# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Matthias Westerhausen Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 07743 Jena Germany ; _publ_contact_author_phone '03641 948 110' _publ_contact_author_fax '03641 948 102' _publ_contact_author_email m.we@uni-jena.de # 3. TITLE AND AUTHOR LIST _publ_section_title ; Substituted Phenylamide Complexes of the Heavy Alkaline Earth Metals Calcium, Strontium and Barium Variations and Limitations ; loop_ _publ_author_name _publ_author_address 'Matthias Westerhausen' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; M.Gartner ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; H.Gorls ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena Lessing-Str. 8 D-07743 Jena Germany ; _publ_contact_author_name 'Matthias Westerhausen' # data_FO3215 _database_code_depnum_ccdc_archive 'CCDC 666447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 F2 K N O4' _chemical_formula_weight 343.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8620(3) _cell_length_b 12.3064(5) _cell_length_c 12.4436(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.024(2) _cell_angle_gamma 90.00 _cell_volume 1654.18(10) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9306 _exptl_absorpt_correction_T_max 0.9688 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11525 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3779 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.7861P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3779 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.62706(4) 0.00429(4) 0.41550(4) 0.03723(17) Uani 1 1 d . . . F1 F 0.54346(19) 0.20091(17) 0.50223(15) 0.0769(6) Uani 1 1 d . . . F2 F 0.21724(18) 0.1841(2) 0.22495(18) 0.0897(7) Uani 1 1 d . . . O1 O 0.72588(16) 0.12294(14) 0.24964(15) 0.0502(5) Uani 1 1 d . . . O2 O 0.82395(16) 0.32509(13) 0.19364(15) 0.0482(4) Uani 1 1 d . . . O3 O 0.87099(15) 0.01106(15) 0.48324(15) 0.0497(5) Uani 1 1 d . . . N1 N 0.3813(2) 0.07419(19) 0.37461(19) 0.0467(6) Uani 1 1 d . . . C1 C 0.3782(2) 0.1834(2) 0.3637(2) 0.0442(6) Uani 1 1 d . . . C2 C 0.4590(3) 0.2516(2) 0.4271(2) 0.0547(7) Uani 1 1 d . . . C3 C 0.4678(4) 0.3662(3) 0.4198(4) 0.0911(14) Uani 1 1 d . . . H3A H 0.5255 0.4081 0.4651 0.109 Uiso 1 1 calc R . . C4 C 0.3817(5) 0.4129(3) 0.3378(4) 0.1073(19) Uani 1 1 d . . . H4A H 0.3815 0.4894 0.3279 0.129 Uiso 1 1 calc R . . C5 C 0.2987(4) 0.3501(3) 0.2725(4) 0.0919(15) Uani 1 1 d . . . H5A H 0.2430 0.3828 0.2179 0.110 Uiso 1 1 calc R . . C6 C 0.2985(3) 0.2430(3) 0.2877(3) 0.0628(8) Uani 1 1 d . . . C7 C 0.8369(2) 0.1303(2) 0.1978(2) 0.0498(6) Uani 1 1 d . . . H7A H 0.8164 0.1250 0.1186 0.060 Uiso 1 1 calc R . . H7B H 0.8921 0.0688 0.2213 0.060 Uiso 1 1 calc R . . C8 C 0.9029(2) 0.2349(2) 0.2246(2) 0.0489(6) Uani 1 1 d . . . H8A H 0.9287 0.2382 0.3032 0.059 Uiso 1 1 calc R . . H8B H 0.9782 0.2388 0.1863 0.059 Uiso 1 1 calc R . . C9 C 0.7135(2) 0.3176(2) 0.2452(2) 0.0513(6) Uani 1 1 d . . . H9A H 0.6585 0.3795 0.2225 0.062 Uiso 1 1 calc R . . H9B H 0.7340 0.3218 0.3245 0.062 Uiso 1 1 calc R . . C10 C 0.6477(2) 0.2132(2) 0.2165(2) 0.0481(6) Uani 1 1 d . . . H10A H 0.5709 0.2094 0.2527 0.058 Uiso 1 1 calc R . . H10B H 0.6245 0.2100 0.1375 0.058 Uiso 1 1 calc R . . C11 C 0.9485(2) 0.1024(2) 0.5094(2) 0.0500(6) Uani 1 1 d . . . H11A H 0.9587 0.1130 0.5887 0.060 Uiso 1 1 calc R . . H11B H 0.9094 0.1685 0.4758 0.060 Uiso 1 1 calc R . . C12 C 1.0732(2) 0.0854(2) 0.4696(2) 0.0500(6) Uani 1 1 d . . . H12A H 1.0637 0.0787 0.3899 0.075 Uiso 1 1 calc R . . H12C H 1.1271 0.1487 0.4895 0.075 Uiso 1 1 calc R . . O4 O 0.47932(18) 0.11198(16) -0.02157(16) 0.0572(5) Uani 1 1 d . . . C13 C 0.4004(3) 0.0506(3) 0.0385(3) 0.0676(8) Uani 1 1 d . . . H13A H 0.3301 0.0223 -0.0108 0.081 Uiso 1 1 calc R . . H13B H 0.3664 0.0982 0.0923 0.081 Uiso 1 1 calc R . . C14 C 0.4681(3) -0.0425(3) 0.0954(3) 0.0677(9) Uani 1 1 d . . . H14A H 0.5345 -0.0139 0.1484 0.081 Uiso 1 1 calc R . . H14B H 0.4100 -0.0846 0.1354 0.081 Uiso 1 1 calc R . . H1N1 H 0.340(4) 0.057(4) 0.338(4) 0.102 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0298(3) 0.0408(3) 0.0418(3) 0.0021(2) 0.00719(19) 0.0046(2) F1 0.0778(12) 0.0833(13) 0.0671(11) -0.0247(10) -0.0049(9) 0.0165(10) F2 0.0603(12) 0.1214(19) 0.0857(15) 0.0236(13) 0.0002(10) 0.0256(12) O1 0.0482(10) 0.0486(10) 0.0551(11) 0.0131(8) 0.0124(8) -0.0051(8) O2 0.0448(9) 0.0395(9) 0.0600(11) 0.0107(8) 0.0046(8) 0.0008(8) O3 0.0305(8) 0.0623(12) 0.0553(11) 0.0143(9) -0.0007(8) -0.0009(8) N1 0.0466(13) 0.0394(11) 0.0549(14) 0.0093(10) 0.0084(10) 0.0100(10) C1 0.0438(13) 0.0407(13) 0.0522(14) 0.0110(11) 0.0245(11) 0.0138(11) C2 0.0546(16) 0.0565(16) 0.0562(16) -0.0060(13) 0.0204(13) 0.0168(14) C3 0.106(3) 0.0586(19) 0.122(3) 0.016(2) 0.079(3) 0.033(2) C4 0.133(4) 0.050(2) 0.157(4) 0.037(3) 0.102(4) 0.038(2) C5 0.096(3) 0.072(2) 0.118(3) 0.055(2) 0.062(3) 0.048(2) C6 0.0485(16) 0.075(2) 0.0685(19) 0.0239(16) 0.0238(15) 0.0210(15) C7 0.0476(14) 0.0438(14) 0.0603(16) 0.0068(12) 0.0161(12) 0.0070(12) C8 0.0400(13) 0.0489(14) 0.0584(16) 0.0140(12) 0.0076(12) 0.0036(11) C9 0.0507(15) 0.0498(15) 0.0539(15) -0.0079(12) 0.0073(12) 0.0076(12) C10 0.0378(13) 0.0600(16) 0.0477(14) 0.0011(12) 0.0103(11) -0.0014(12) C11 0.0426(13) 0.0527(15) 0.0550(16) 0.0083(12) 0.0063(11) -0.0009(12) C12 0.0410(13) 0.0550(15) 0.0541(15) 0.0118(13) 0.0049(11) -0.0071(12) O4 0.0665(12) 0.0481(11) 0.0581(12) -0.0005(9) 0.0114(10) 0.0011(9) C13 0.0636(19) 0.069(2) 0.075(2) 0.0021(16) 0.0262(16) 0.0102(16) C14 0.084(2) 0.0656(18) 0.0582(18) 0.0081(15) 0.0285(16) 0.0078(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O2 2.6726(17) 2_645 ? K1 O3 2.6961(17) . ? K1 N1 2.795(2) 3_656 ? K1 N1 2.800(2) . ? K1 O1 2.8300(17) . ? K1 F1 2.8372(19) . ? K1 F1 3.355(2) 3_656 ? K1 C1 3.495(2) . ? K1 K1 3.6428(9) 3_656 ? F1 C2 1.387(3) . ? F1 K1 3.355(2) 3_656 ? F2 C6 1.330(4) . ? O1 C7 1.429(3) . ? O1 C10 1.432(3) . ? O2 C9 1.422(3) . ? O2 C8 1.430(3) . ? O2 K1 2.6726(17) 2_655 ? O3 C11 1.421(3) . ? O3 C12 1.430(3) 3_756 ? N1 C1 1.351(3) . ? N1 K1 2.795(2) 3_656 ? N1 H1N1 0.64(4) . ? C1 C2 1.398(4) . ? C1 C6 1.418(4) . ? C2 C3 1.417(4) . ? C3 C4 1.430(7) . ? C3 H3A 0.9500 . ? C4 C5 1.385(7) . ? C4 H4A 0.9500 . ? C5 C6 1.332(5) . ? C5 H5A 0.9500 . ? C7 C8 1.494(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.505(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.430(3) 3_756 ? C12 H12A 0.9900 . ? C12 H12C 0.9900 . ? O4 C13 1.414(4) . ? O4 C14 1.418(3) 3_655 ? C13 C14 1.499(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.418(3) 3_655 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 K1 O3 86.72(6) 2_645 . ? O2 K1 N1 102.56(6) 2_645 3_656 ? O3 K1 N1 81.12(6) . 3_656 ? O2 K1 N1 113.46(6) 2_645 . ? O3 K1 N1 159.11(7) . . ? N1 K1 N1 98.76(6) 3_656 . ? O2 K1 O1 86.80(5) 2_645 . ? O3 K1 O1 77.09(5) . . ? N1 K1 O1 155.74(6) 3_656 . ? N1 K1 O1 97.84(6) . . ? O2 K1 F1 170.32(6) 2_645 . ? O3 K1 F1 101.42(6) . . ? N1 K1 F1 84.04(6) 3_656 . ? N1 K1 F1 58.00(6) . . ? O1 K1 F1 89.91(6) . . ? O2 K1 F1 71.32(5) 2_645 3_656 ? O3 K1 F1 118.94(5) . 3_656 ? N1 K1 F1 51.81(6) 3_656 3_656 ? N1 K1 F1 74.95(6) . 3_656 ? O1 K1 F1 151.02(5) . 3_656 ? F1 K1 F1 108.48(5) . 3_656 ? O2 K1 C1 128.17(6) 2_645 . ? O3 K1 C1 138.93(6) . . ? N1 K1 C1 106.87(6) 3_656 . ? N1 K1 C1 21.34(7) . . ? O1 K1 C1 83.41(5) . . ? F1 K1 C1 42.28(6) . . ? F1 K1 C1 95.16(5) 3_656 . ? O2 K1 K1 118.21(4) 2_645 3_656 ? O3 K1 K1 126.85(5) . 3_656 ? N1 K1 K1 49.44(5) 3_656 3_656 ? N1 K1 K1 49.31(5) . 3_656 ? O1 K1 K1 143.55(4) . 3_656 ? F1 K1 K1 60.86(5) . 3_656 ? F1 K1 K1 47.62(3) 3_656 3_656 ? C1 K1 K1 60.44(4) . 3_656 ? C2 F1 K1 110.03(14) . . ? C2 F1 K1 101.37(16) . 3_656 ? K1 F1 K1 71.52(5) . 3_656 ? C7 O1 C10 108.93(17) . . ? C7 O1 K1 139.85(15) . . ? C10 O1 K1 110.54(13) . . ? C9 O2 C8 109.79(18) . . ? C9 O2 K1 120.34(14) . 2_655 ? C8 O2 K1 129.16(14) . 2_655 ? C11 O3 C12 110.31(19) . 3_756 ? C11 O3 K1 129.43(15) . . ? C12 O3 K1 117.55(14) 3_756 . ? C1 N1 K1 115.79(17) . 3_656 ? C1 N1 K1 109.69(17) . . ? K1 N1 K1 81.24(6) 3_656 . ? C1 N1 H1N1 104(4) . . ? K1 N1 H1N1 118(4) 3_656 . ? K1 N1 H1N1 128(4) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 C6 126.1(3) . . ? C2 C1 C6 111.7(3) . . ? N1 C1 K1 48.97(13) . . ? C2 C1 K1 81.17(15) . . ? C6 C1 K1 148.88(17) . . ? F1 C2 C1 116.3(2) . . ? F1 C2 C3 116.5(3) . . ? C1 C2 C3 127.2(3) . . ? C2 C3 C4 113.7(4) . . ? C2 C3 H3A 123.1 . . ? C4 C3 H3A 123.1 . . ? C5 C4 C3 122.1(3) . . ? C5 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 H5A 120.7 . . ? C4 C5 H5A 120.7 . . ? C5 C6 F2 117.8(3) . . ? C5 C6 C1 126.7(4) . . ? F2 C6 C1 115.5(3) . . ? O1 C7 C8 111.2(2) . . ? O1 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? O1 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O2 C8 C7 110.4(2) . . ? O2 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O2 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C10 110.7(2) . . ? O2 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O1 C10 C9 110.1(2) . . ? O1 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O1 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? O3 C11 C12 110.3(2) . . ? O3 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? O3 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O3 C12 C11 109.7(2) 3_756 . ? O3 C12 H12A 109.7 3_756 . ? C11 C12 H12A 109.7 . . ? O3 C12 H12C 109.7 3_756 . ? C11 C12 H12C 109.7 . . ? H12A C12 H12C 108.2 . . ? C13 O4 C14 109.2(2) . 3_655 ? O4 C13 C14 111.3(2) . . ? O4 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? O4 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? O4 C14 C13 111.5(3) 3_655 . ? O4 C14 H14A 109.3 3_655 . ? C13 C14 H14A 109.3 . . ? O4 C14 H14B 109.3 3_655 . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.696 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.057 #==== END data_FO3228 _database_code_depnum_ccdc_archive 'CCDC 666448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Ca N2 O4' _chemical_formula_weight 540.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7482(10) _cell_length_b 17.8861(11) _cell_length_c 20.6278(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6179.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9434 _exptl_absorpt_correction_T_max 0.9884 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19352 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.44 _reflns_number_total 6636 _reflns_number_gt 4035 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+3.7556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6636 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.28553(3) 0.05638(3) 0.13380(2) 0.02352(14) Uani 1 1 d . . . O1 O 0.14155(11) 0.06628(11) 0.13461(10) 0.0381(5) Uani 1 1 d . . . O2 O 0.26965(10) -0.04516(10) 0.21093(8) 0.0315(4) Uani 1 1 d . . . O3 O 0.42658(10) 0.03914(10) 0.13502(8) 0.0291(4) Uani 1 1 d . . . O4 O 0.29760(11) 0.16267(10) 0.06359(8) 0.0342(5) Uani 1 1 d . . . N1 N 0.29688(12) 0.13562(12) 0.22733(10) 0.0274(5) Uani 1 1 d . . . N2 N 0.27370(13) -0.02353(13) 0.03918(10) 0.0306(5) Uani 1 1 d . . . C1 C 0.35036(15) 0.18849(14) 0.24689(12) 0.0264(6) Uani 1 1 d . . . C2 C 0.41708(15) 0.20517(15) 0.20714(13) 0.0312(6) Uani 1 1 d . . . H2A H 0.4243 0.1778 0.1681 0.037 Uiso 1 1 calc R . . C3 C 0.47153(16) 0.25926(17) 0.22288(15) 0.0411(7) Uani 1 1 d . . . H3A H 0.5155 0.2681 0.1948 0.049 Uiso 1 1 calc R . . C4 C 0.46372(17) 0.30167(18) 0.27931(16) 0.0441(8) Uani 1 1 d . . . H4A H 0.5012 0.3397 0.2899 0.053 Uiso 1 1 calc R . . C5 C 0.39992(18) 0.28647(17) 0.31911(14) 0.0392(7) Uani 1 1 d . . . H5A H 0.3933 0.3148 0.3577 0.047 Uiso 1 1 calc R . . C6 C 0.34510(16) 0.23126(16) 0.30468(13) 0.0323(6) Uani 1 1 d . . . H6A H 0.3028 0.2217 0.3342 0.039 Uiso 1 1 calc R . . C7 C 0.23127(16) 0.12361(16) 0.27241(13) 0.0329(6) Uani 1 1 d . . . H7A H 0.2526 0.1083 0.3146 0.049 Uiso 1 1 calc R . . H7B H 0.1961 0.0844 0.2556 0.049 Uiso 1 1 calc R . . H7C H 0.2009 0.1701 0.2774 0.049 Uiso 1 1 calc R . . C8 C 0.31351(15) -0.08570(15) 0.01976(12) 0.0270(6) Uani 1 1 d . . . C9 C 0.37274(15) -0.11777(15) 0.06079(13) 0.0282(6) Uani 1 1 d . . . H9A H 0.3827 -0.0952 0.1017 0.034 Uiso 1 1 calc R . . C10 C 0.41606(15) -0.17992(16) 0.04376(14) 0.0329(6) Uani 1 1 d . . . H10A H 0.4553 -0.1985 0.0728 0.039 Uiso 1 1 calc R . . C11 C 0.40373(18) -0.21634(17) -0.01519(15) 0.0391(7) Uani 1 1 d . . . H11A H 0.4336 -0.2595 -0.0268 0.047 Uiso 1 1 calc R . . C12 C 0.34617(18) -0.18707(17) -0.05613(14) 0.0395(7) Uani 1 1 d . . . H12A H 0.3368 -0.2106 -0.0967 0.047 Uiso 1 1 calc R . . C13 C 0.30185(16) -0.12459(16) -0.03972(13) 0.0333(6) Uani 1 1 d . . . H13A H 0.2624 -0.1071 -0.0691 0.040 Uiso 1 1 calc R . . C14 C 0.21443(18) 0.00340(18) -0.00715(14) 0.0408(7) Uani 1 1 d . . . H14A H 0.1745 -0.0357 -0.0147 0.061 Uiso 1 1 calc R . . H14B H 0.2408 0.0159 -0.0481 0.061 Uiso 1 1 calc R . . H14C H 0.1882 0.0480 0.0103 0.061 Uiso 1 1 calc R . . C15 C 0.0958(2) 0.1346(2) 0.1333(2) 0.0728(12) Uani 1 1 d . . . H15A H 0.0952 0.1578 0.1769 0.087 Uiso 1 1 calc R . . H15B H 0.1197 0.1704 0.1024 0.087 Uiso 1 1 calc R . . C16 C 0.0158(2) 0.1160(3) 0.1136(3) 0.1012(18) Uani 1 1 d . . . H16A H 0.0039 0.1390 0.0710 0.121 Uiso 1 1 calc R . . H16B H -0.0231 0.1353 0.1456 0.121 Uiso 1 1 calc R . . C17 C 0.0097(2) 0.0349(3) 0.1091(2) 0.0817(14) Uani 1 1 d . . . H17A H -0.0005 0.0195 0.0638 0.098 Uiso 1 1 calc R . . H17B H -0.0347 0.0165 0.1365 0.098 Uiso 1 1 calc R . . C18 C 0.08756(18) 0.00353(19) 0.13234(16) 0.0472(8) Uani 1 1 d . . . H18A H 0.0815 -0.0191 0.1759 0.057 Uiso 1 1 calc R . . H18B H 0.1075 -0.0351 0.1020 0.057 Uiso 1 1 calc R . . C19 C 0.24566(17) -0.12010(15) 0.19302(13) 0.0326(6) Uani 1 1 d . . . H19A H 0.2462 -0.1264 0.1453 0.039 Uiso 1 1 calc R . . H19B H 0.1915 -0.1315 0.2094 0.039 Uiso 1 1 calc R . . C20 C 0.30754(17) -0.16990(16) 0.22492(14) 0.0372(7) Uani 1 1 d . . . H20A H 0.3554 -0.1755 0.1971 0.045 Uiso 1 1 calc R . . H20B H 0.2853 -0.2200 0.2344 0.045 Uiso 1 1 calc R . . C21 C 0.32749(19) -0.12777(18) 0.28738(15) 0.0441(8) Uani 1 1 d . . . H21A H 0.3037 -0.1532 0.3254 0.053 Uiso 1 1 calc R . . H21B H 0.3860 -0.1245 0.2936 0.053 Uiso 1 1 calc R . . C22 C 0.29154(17) -0.05022(17) 0.27852(12) 0.0353(6) Uani 1 1 d . . . H22A H 0.2440 -0.0440 0.3065 0.042 Uiso 1 1 calc R . . H22B H 0.3310 -0.0111 0.2898 0.042 Uiso 1 1 calc R . . C23 C 0.47945(16) 0.03874(17) 0.07945(13) 0.0350(7) Uani 1 1 d . . . H23A H 0.4959 0.0902 0.0680 0.042 Uiso 1 1 calc R . . H23B H 0.4529 0.0157 0.0415 0.042 Uiso 1 1 calc R . . C24 C 0.55048(16) -0.00704(18) 0.10032(14) 0.0403(7) Uani 1 1 d . . . H24A H 0.5990 0.0067 0.0757 0.048 Uiso 1 1 calc R . . H24B H 0.5403 -0.0613 0.0953 0.048 Uiso 1 1 calc R . . C25 C 0.55756(17) 0.01490(19) 0.17142(15) 0.0443(8) Uani 1 1 d . . . H25A H 0.5870 -0.0235 0.1964 0.053 Uiso 1 1 calc R . . H25B H 0.5848 0.0637 0.1764 0.053 Uiso 1 1 calc R . . C26 C 0.47125(16) 0.01950(17) 0.19267(13) 0.0345(7) Uani 1 1 d . . . H26A H 0.4530 -0.0292 0.2101 0.041 Uiso 1 1 calc R . . H26B H 0.4645 0.0581 0.2266 0.041 Uiso 1 1 calc R . . C27 C 0.28580(16) 0.23894(15) 0.08439(13) 0.0313(6) Uani 1 1 d . . . H27A H 0.2885 0.2427 0.1322 0.038 Uiso 1 1 calc R . . H27B H 0.2333 0.2578 0.0697 0.038 Uiso 1 1 calc R . . C28 C 0.35255(17) 0.28262(17) 0.05349(14) 0.0396(7) Uani 1 1 d . . . H28A H 0.4004 0.2833 0.0816 0.047 Uiso 1 1 calc R . . H28B H 0.3359 0.3347 0.0444 0.047 Uiso 1 1 calc R . . C29 C 0.3686(2) 0.2403(2) -0.00877(16) 0.0526(9) Uani 1 1 d . . . H29A H 0.3497 0.2693 -0.0467 0.063 Uiso 1 1 calc R . . H29B H 0.4264 0.2304 -0.0138 0.063 Uiso 1 1 calc R . . C30 C 0.3230(2) 0.16807(19) -0.00286(14) 0.0522(9) Uani 1 1 d . . . H30A H 0.2763 0.1682 -0.0322 0.063 Uiso 1 1 calc R . . H30B H 0.3577 0.1252 -0.0143 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0272(3) 0.0199(3) 0.0234(3) -0.0005(2) -0.0012(2) -0.0006(2) O1 0.0315(10) 0.0320(12) 0.0507(12) -0.0005(9) -0.0033(9) 0.0030(8) O2 0.0412(11) 0.0236(11) 0.0296(10) 0.0031(8) -0.0033(8) -0.0027(8) O3 0.0281(9) 0.0337(11) 0.0254(9) -0.0028(8) 0.0002(8) 0.0007(7) O4 0.0487(12) 0.0250(11) 0.0290(10) 0.0035(8) 0.0064(9) 0.0059(8) N1 0.0310(12) 0.0255(13) 0.0258(11) -0.0028(9) 0.0050(9) -0.0052(9) N2 0.0376(13) 0.0276(13) 0.0266(11) -0.0013(9) -0.0055(10) 0.0021(10) C1 0.0301(14) 0.0214(14) 0.0275(14) 0.0024(11) -0.0024(11) 0.0004(11) C2 0.0331(15) 0.0270(16) 0.0337(15) -0.0034(12) 0.0026(12) -0.0014(11) C3 0.0293(15) 0.0394(19) 0.0545(19) 0.0002(15) -0.0003(14) -0.0067(13) C4 0.0381(17) 0.0386(19) 0.056(2) -0.0131(15) -0.0099(15) -0.0095(13) C5 0.0466(18) 0.0338(17) 0.0371(16) -0.0103(13) -0.0090(14) -0.0010(13) C6 0.0335(15) 0.0344(17) 0.0289(14) -0.0007(12) -0.0015(12) -0.0003(12) C7 0.0404(16) 0.0286(16) 0.0297(14) -0.0013(12) 0.0069(12) -0.0052(12) C8 0.0313(14) 0.0264(15) 0.0233(13) -0.0005(11) -0.0005(11) -0.0098(11) C9 0.0292(14) 0.0282(15) 0.0272(14) -0.0021(11) 0.0020(11) -0.0087(11) C10 0.0289(14) 0.0329(17) 0.0369(16) 0.0023(12) 0.0007(12) -0.0053(12) C11 0.0420(17) 0.0293(17) 0.0461(18) -0.0085(13) 0.0093(14) -0.0019(13) C12 0.0523(18) 0.0352(18) 0.0311(16) -0.0112(13) 0.0045(14) -0.0098(14) C13 0.0416(16) 0.0322(16) 0.0261(14) 0.0006(12) -0.0025(12) -0.0061(12) C14 0.0505(18) 0.0381(18) 0.0339(16) -0.0018(13) -0.0090(14) 0.0043(14) C15 0.051(2) 0.042(2) 0.125(4) -0.007(2) -0.018(2) 0.0189(17) C16 0.048(2) 0.072(3) 0.184(6) 0.031(3) -0.006(3) 0.016(2) C17 0.046(2) 0.089(4) 0.110(4) 0.004(3) -0.028(2) -0.005(2) C18 0.0411(17) 0.044(2) 0.056(2) 0.0022(16) -0.0025(15) -0.0048(14) C19 0.0358(15) 0.0240(16) 0.0379(16) 0.0019(12) 0.0009(13) -0.0044(12) C20 0.0384(16) 0.0250(16) 0.0480(18) 0.0050(13) 0.0016(13) 0.0006(12) C21 0.0487(18) 0.0405(19) 0.0429(18) 0.0082(14) -0.0085(15) 0.0041(14) C22 0.0410(16) 0.0396(18) 0.0252(14) 0.0043(12) -0.0002(12) 0.0003(13) C23 0.0360(15) 0.0391(18) 0.0298(15) 0.0006(12) 0.0063(12) -0.0094(12) C24 0.0253(14) 0.048(2) 0.0476(18) 0.0006(15) 0.0082(13) -0.0053(13) C25 0.0314(16) 0.052(2) 0.0495(19) 0.0016(16) -0.0100(14) -0.0084(14) C26 0.0381(16) 0.0368(17) 0.0287(15) 0.0008(12) -0.0051(12) 0.0046(13) C27 0.0387(15) 0.0232(15) 0.0322(14) 0.0015(11) 0.0026(12) 0.0078(12) C28 0.0414(17) 0.0362(18) 0.0411(17) 0.0086(14) -0.0002(14) -0.0019(13) C29 0.050(2) 0.057(2) 0.050(2) 0.0049(17) 0.0175(16) -0.0001(16) C30 0.088(3) 0.042(2) 0.0260(16) 0.0027(14) 0.0123(16) 0.0070(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O3 2.3825(17) . ? Ca O4 2.3985(18) . ? Ca N1 2.402(2) . ? Ca O1 2.4180(18) . ? Ca N2 2.427(2) . ? Ca O2 2.4291(18) . ? O1 C18 1.442(3) . ? O1 C15 1.442(4) . ? O2 C22 1.444(3) . ? O2 C19 1.447(3) . ? O3 C26 1.448(3) . ? O3 C23 1.448(3) . ? O4 C30 1.439(3) . ? O4 C27 1.444(3) . ? N1 C1 1.363(3) . ? N1 C7 1.455(3) . ? N2 C8 1.357(3) . ? N2 C14 1.460(3) . ? C1 C2 1.418(4) . ? C1 C6 1.419(4) . ? C2 C3 1.369(4) . ? C3 C4 1.396(4) . ? C4 C5 1.375(4) . ? C5 C6 1.381(4) . ? C8 C13 1.424(4) . ? C8 C9 1.424(4) . ? C9 C10 1.373(4) . ? C10 C11 1.395(4) . ? C11 C12 1.385(4) . ? C12 C13 1.384(4) . ? C15 C16 1.439(5) . ? C16 C17 1.458(6) . ? C17 C18 1.499(5) . ? C19 C20 1.517(4) . ? C20 C21 1.529(4) . ? C21 C22 1.523(4) . ? C23 C24 1.507(4) . ? C24 C25 1.523(4) . ? C25 C26 1.513(4) . ? C27 C28 1.505(4) . ? C28 C29 1.515(4) . ? C29 C30 1.505(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ca O4 91.45(6) . . ? O3 Ca N1 89.39(7) . . ? O4 Ca N1 90.61(7) . . ? O3 Ca O1 176.62(7) . . ? O4 Ca O1 91.73(7) . . ? N1 Ca O1 91.73(7) . . ? O3 Ca N2 90.76(7) . . ? O4 Ca N2 89.32(7) . . ? N1 Ca N2 179.84(8) . . ? O1 Ca N2 88.13(7) . . ? O3 Ca O2 90.28(6) . . ? O4 Ca O2 175.84(6) . . ? N1 Ca O2 85.62(7) . . ? O1 Ca O2 86.62(6) . . ? N2 Ca O2 94.45(7) . . ? C18 O1 C15 109.0(2) . . ? C18 O1 Ca 124.61(16) . . ? C15 O1 Ca 126.32(19) . . ? C22 O2 C19 105.00(19) . . ? C22 O2 Ca 130.65(16) . . ? C19 O2 Ca 123.75(15) . . ? C26 O3 C23 109.44(19) . . ? C26 O3 Ca 123.53(14) . . ? C23 O3 Ca 126.75(15) . . ? C30 O4 C27 105.1(2) . . ? C30 O4 Ca 130.81(17) . . ? C27 O4 Ca 123.92(14) . . ? C1 N1 C7 114.2(2) . . ? C1 N1 Ca 134.35(16) . . ? C7 N1 Ca 111.49(16) . . ? C8 N2 C14 114.3(2) . . ? C8 N2 Ca 132.83(16) . . ? C14 N2 Ca 112.81(17) . . ? N1 C1 C2 119.5(2) . . ? N1 C1 C6 125.6(2) . . ? C2 C1 C6 114.9(2) . . ? C3 C2 C1 122.5(3) . . ? C2 C3 C4 121.3(3) . . ? C5 C4 C3 117.6(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 121.7(3) . . ? N2 C8 C13 126.0(2) . . ? N2 C8 C9 119.8(2) . . ? C13 C8 C9 114.3(2) . . ? C10 C9 C8 122.8(2) . . ? C9 C10 C11 121.5(3) . . ? C12 C11 C10 117.3(3) . . ? C13 C12 C11 122.0(3) . . ? C12 C13 C8 122.1(3) . . ? C16 C15 O1 107.8(3) . . ? C15 C16 C17 108.2(3) . . ? C16 C17 C18 106.9(3) . . ? O1 C18 C17 105.4(3) . . ? O2 C19 C20 104.1(2) . . ? C19 C20 C21 103.0(2) . . ? C22 C21 C20 105.2(2) . . ? O2 C22 C21 105.9(2) . . ? O3 C23 C24 105.0(2) . . ? C23 C24 C25 101.3(2) . . ? C26 C25 C24 102.6(2) . . ? O3 C26 C25 105.6(2) . . ? O4 C27 C28 105.2(2) . . ? C27 C28 C29 103.4(2) . . ? C30 C29 C28 105.7(2) . . ? O4 C30 C29 106.6(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.340 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.054 #==== END data_FO3189 _database_code_depnum_ccdc_archive 'CCDC 666449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H118 Ca3 N6 O6' _chemical_formula_weight 1356.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.418(3) _cell_length_b 12.619(3) _cell_length_c 12.762(3) _cell_angle_alpha 86.198(3) _cell_angle_beta 87.461(3) _cell_angle_gamma 87.973(3) _cell_volume 1992.4(7) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9233 _exptl_absorpt_correction_T_max 0.9783 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6705 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.02 _reflns_number_total 5061 _reflns_number_gt 3108 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1325P)^2^+4.5641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5061 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2872 _refine_ls_wR_factor_gt 0.2339 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.64884(9) 0.14895(10) 0.14901(10) 0.0392(4) Uani 1 1 d . . . Ca2 Ca 0.5000 0.0000 0.0000 0.0394(5) Uani 1 2 d S . . O1 O 0.7539(4) 0.1047(4) 0.3109(4) 0.0591(13) Uani 1 1 d . . . O2 O 0.6049(4) 0.3116(4) 0.2538(4) 0.0579(13) Uani 1 1 d . . . O3 O 0.8120(4) 0.2530(4) 0.1053(4) 0.0589(13) Uani 1 1 d . . . N1 N 0.4571(4) 0.1676(4) 0.1057(4) 0.0455(13) Uani 1 1 d . . . H1A H 0.4638 0.2190 0.0503 0.055 Uiso 1 1 calc R . . N2 N 0.6670(4) 0.1062(4) -0.0428(4) 0.0449(13) Uani 1 1 d . . . H2A H 0.7180 0.0506 -0.0360 0.054 Uiso 1 1 calc R . . N3 N 0.6063(4) -0.0427(4) 0.1676(4) 0.0460(13) Uani 1 1 d . . . H3B H 0.5489 -0.0382 0.2166 0.055 Uiso 1 1 calc R . . C1 C 0.3701(5) 0.2151(5) 0.1614(6) 0.0477(16) Uani 1 1 d . . . C2 C 0.3020(5) 0.2960(6) 0.1131(7) 0.0592(19) Uani 1 1 d . . . C3 C 0.2144(6) 0.3403(7) 0.1739(8) 0.076(2) Uani 1 1 d . . . H3A H 0.1700 0.3941 0.1406 0.091 Uiso 1 1 calc R . . C4 C 0.1904(6) 0.3104(8) 0.2772(8) 0.076(2) Uani 1 1 d . . . C5 C 0.2579(6) 0.2354(7) 0.3262(7) 0.067(2) Uani 1 1 d . . . H5A H 0.2457 0.2161 0.3989 0.081 Uiso 1 1 calc R . . C6 C 0.3456(5) 0.1864(6) 0.2700(6) 0.0577(18) Uani 1 1 d . . . C7 C 0.3213(7) 0.3367(8) 0.0001(7) 0.081(3) Uani 1 1 d . . . H7A H 0.3282 0.2765 -0.0448 0.122 Uiso 1 1 calc R . . H7B H 0.3877 0.3766 -0.0065 0.122 Uiso 1 1 calc R . . H7C H 0.2604 0.3833 -0.0217 0.122 Uiso 1 1 calc R . . C8 C 0.0906(8) 0.3581(11) 0.3417(10) 0.120(4) Uani 1 1 d . . . H8A H 0.0252 0.3539 0.3020 0.179 Uiso 1 1 calc R . . H8B H 0.1029 0.4326 0.3535 0.179 Uiso 1 1 calc R . . H8C H 0.0816 0.3176 0.4095 0.179 Uiso 1 1 calc R . . C9 C 0.4120(7) 0.1006(8) 0.3253(7) 0.089(3) Uani 1 1 d . . . H9A H 0.3868 0.0917 0.3991 0.133 Uiso 1 1 calc R . . H9B H 0.4879 0.1202 0.3214 0.133 Uiso 1 1 calc R . . H9C H 0.4050 0.0338 0.2916 0.133 Uiso 1 1 calc R . . C10 C 0.7150(5) 0.1617(6) -0.1305(5) 0.0460(16) Uani 1 1 d . . . C11 C 0.7971(6) 0.1133(7) -0.2000(6) 0.058(2) Uani 1 1 d . . . C12 C 0.8414(7) 0.1718(8) -0.2863(6) 0.079(3) Uani 1 1 d . . . H12A H 0.8942 0.1385 -0.3305 0.095 Uiso 1 1 calc R . . C13 C 0.8109(7) 0.2778(9) -0.3102(7) 0.080(3) Uani 1 1 d . . . C14 C 0.7348(7) 0.3259(7) -0.2415(7) 0.073(3) Uani 1 1 d . . . H14A H 0.7155 0.3988 -0.2553 0.088 Uiso 1 1 calc R . . C15 C 0.6863(5) 0.2706(6) -0.1537(6) 0.0572(19) Uani 1 1 d . . . C16 C 0.8371(6) 0.0007(7) -0.1781(7) 0.077(2) Uani 1 1 d . . . H16A H 0.8819 -0.0218 -0.2383 0.116 Uiso 1 1 calc R . . H16B H 0.7755 -0.0457 -0.1665 0.116 Uiso 1 1 calc R . . H16C H 0.8800 -0.0038 -0.1153 0.116 Uiso 1 1 calc R . . C17 C 0.8554(10) 0.3405(10) -0.4085(8) 0.119(4) Uani 1 1 d . . . H17A H 0.8575 0.2955 -0.4683 0.179 Uiso 1 1 calc R . . H17B H 0.9284 0.3626 -0.3965 0.179 Uiso 1 1 calc R . . H17C H 0.8087 0.4034 -0.4235 0.179 Uiso 1 1 calc R . . C18 C 0.6017(7) 0.3261(8) -0.0879(8) 0.086(3) Uani 1 1 d . . . H18A H 0.6022 0.4027 -0.1065 0.129 Uiso 1 1 calc R . . H18B H 0.6168 0.3126 -0.0134 0.129 Uiso 1 1 calc R . . H18C H 0.5307 0.2993 -0.1009 0.129 Uiso 1 1 calc R . . C19 C 0.6617(5) -0.1310(5) 0.2156(5) 0.0467(16) Uani 1 1 d . . . C20 C 0.6141(6) -0.1992(6) 0.2964(6) 0.059(2) Uani 1 1 d . . . C21 C 0.6741(8) -0.2870(7) 0.3397(7) 0.077(3) Uani 1 1 d . . . H21A H 0.6396 -0.3325 0.3922 0.092 Uiso 1 1 calc R . . C22 C 0.7791(8) -0.3106(6) 0.3107(7) 0.076(3) Uani 1 1 d . . . C23 C 0.8262(6) -0.2411(7) 0.2361(7) 0.068(2) Uani 1 1 d . . . H23A H 0.9002 -0.2531 0.2168 0.082 Uiso 1 1 calc R . . C24 C 0.7718(6) -0.1539(6) 0.1869(6) 0.0576(19) Uani 1 1 d . . . C25 C 0.8390(10) -0.4074(9) 0.3584(10) 0.122(5) Uani 1 1 d . . . H25A H 0.8018 -0.4321 0.4244 0.183 Uiso 1 1 calc R . . H25B H 0.9127 -0.3887 0.3725 0.183 Uiso 1 1 calc R . . H25C H 0.8414 -0.4640 0.3093 0.183 Uiso 1 1 calc R . . C26 C 0.4999(6) -0.1789(7) 0.3374(7) 0.079(3) Uani 1 1 d . . . H26A H 0.4760 -0.2408 0.3817 0.118 Uiso 1 1 calc R . . H26B H 0.4525 -0.1666 0.2781 0.118 Uiso 1 1 calc R . . H26C H 0.4970 -0.1163 0.3790 0.118 Uiso 1 1 calc R . . C27 C 0.8256(7) -0.0870(8) 0.1013(8) 0.086(3) Uani 1 1 d . . . H27A H 0.9029 -0.1056 0.0976 0.128 Uiso 1 1 calc R . . H27B H 0.8152 -0.0119 0.1157 0.128 Uiso 1 1 calc R . . H27C H 0.7943 -0.0994 0.0342 0.128 Uiso 1 1 calc R . . C28 C 0.8647(7) 0.1226(11) 0.3204(9) 0.120(5) Uani 1 1 d . . . H28A H 0.9057 0.1716 0.2767 0.144 Uiso 1 1 calc R . . C29 C 0.9062(8) 0.0553(13) 0.4061(9) 0.138(6) Uani 1 1 d . . . H29A H 0.9331 0.0990 0.4604 0.165 Uiso 1 1 calc R . . H29B H 0.9664 0.0090 0.3805 0.165 Uiso 1 1 calc R . . C30 C 0.8172(9) -0.0088(11) 0.4498(10) 0.125(5) Uani 1 1 d . . . H30A H 0.8137 -0.0101 0.5275 0.150 Uiso 1 1 calc R . . H30B H 0.8259 -0.0827 0.4283 0.150 Uiso 1 1 calc R . . C31 C 0.7197(6) 0.0430(7) 0.4065(6) 0.069(2) Uani 1 1 d . . . H31A H 0.6678 -0.0108 0.3903 0.083 Uiso 1 1 calc R . . H31B H 0.6844 0.0902 0.4577 0.083 Uiso 1 1 calc R . . C32 C 0.5430(7) 0.4064(6) 0.2179(7) 0.067(2) Uani 1 1 d . . . H32A H 0.4882 0.3883 0.1685 0.081 Uiso 1 1 calc R . . H32B H 0.5910 0.4596 0.1819 0.081 Uiso 1 1 calc R . . C33 C 0.4894(10) 0.4495(10) 0.3153(9) 0.111(4) Uani 1 1 d . . . H33A H 0.4144 0.4253 0.3252 0.133 Uiso 1 1 calc R . . H33B H 0.4879 0.5281 0.3101 0.133 Uiso 1 1 calc R . . C34 C 0.5565(12) 0.4064(11) 0.4063(9) 0.137(5) Uani 1 1 d . . . H34A H 0.6011 0.4627 0.4308 0.164 Uiso 1 1 calc R . . H34B H 0.5097 0.3785 0.4658 0.164 Uiso 1 1 calc R . . C35 C 0.6255(11) 0.3203(10) 0.3636(8) 0.111(4) Uani 1 1 d . . . H35A H 0.7024 0.3356 0.3710 0.133 Uiso 1 1 calc R . . H35B H 0.6103 0.2522 0.4036 0.133 Uiso 1 1 calc R . . C36 C 0.9070(6) 0.2193(7) 0.0429(6) 0.067(2) Uani 1 1 d . . . H36A H 0.9612 0.1833 0.0889 0.080 Uiso 1 1 calc R . . H36B H 0.8869 0.1694 -0.0091 0.080 Uiso 1 1 calc R . . C37 C 0.9505(9) 0.3154(10) -0.0102(10) 0.114(4) Uani 1 1 d . . . H37A H 0.9254 0.3258 -0.0828 0.136 Uiso 1 1 calc R . . H37B H 1.0303 0.3120 -0.0126 0.136 Uiso 1 1 calc R . . C38 C 0.9063(9) 0.4056(9) 0.0572(12) 0.130(5) Uani 1 1 d . . . H38A H 0.9642 0.4309 0.0993 0.156 Uiso 1 1 calc R . . H38B H 0.8789 0.4661 0.0115 0.156 Uiso 1 1 calc R . . C39 C 0.8222(9) 0.3644(8) 0.1240(11) 0.114(4) Uani 1 1 d . . . H39A H 0.7537 0.4040 0.1093 0.137 Uiso 1 1 calc R . . H39B H 0.8384 0.3718 0.1983 0.137 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0407(7) 0.0389(7) 0.0377(8) 0.0012(5) -0.0031(5) -0.0011(5) Ca2 0.0417(9) 0.0384(10) 0.0377(10) 0.0016(8) -0.0029(7) -0.0011(7) O1 0.059(3) 0.065(3) 0.053(3) 0.006(3) -0.017(2) -0.003(2) O2 0.067(3) 0.052(3) 0.056(3) -0.016(2) -0.003(2) 0.012(2) O3 0.053(3) 0.060(3) 0.063(3) 0.003(3) 0.005(2) -0.015(2) N1 0.045(3) 0.040(3) 0.051(3) -0.002(2) 0.002(2) 0.004(2) N2 0.041(3) 0.051(3) 0.041(3) 0.007(3) 0.000(2) 0.000(2) N3 0.061(3) 0.034(3) 0.042(3) 0.001(2) -0.002(2) 0.006(2) C1 0.044(3) 0.048(4) 0.053(4) -0.011(3) 0.001(3) -0.006(3) C2 0.043(4) 0.051(4) 0.084(6) -0.016(4) -0.009(3) 0.016(3) C3 0.058(5) 0.072(6) 0.099(8) -0.019(5) -0.011(4) 0.015(4) C4 0.053(5) 0.076(6) 0.101(8) -0.033(5) 0.008(4) 0.011(4) C5 0.069(5) 0.071(6) 0.064(5) -0.017(4) 0.018(4) -0.014(4) C6 0.051(4) 0.057(5) 0.064(5) -0.012(4) 0.007(3) 0.005(3) C7 0.081(6) 0.076(6) 0.085(7) 0.006(5) -0.025(4) 0.024(4) C8 0.088(7) 0.128(11) 0.142(11) -0.050(8) 0.027(7) 0.032(6) C9 0.091(6) 0.100(8) 0.068(6) 0.026(5) 0.029(5) 0.002(5) C10 0.051(4) 0.054(4) 0.034(4) -0.003(3) -0.003(3) -0.009(3) C11 0.053(4) 0.077(6) 0.044(4) -0.005(4) 0.006(3) -0.023(4) C12 0.076(5) 0.103(8) 0.057(6) 0.000(5) 0.018(4) -0.031(5) C13 0.076(6) 0.110(8) 0.054(5) 0.006(5) 0.015(4) -0.037(5) C14 0.075(5) 0.074(6) 0.069(6) 0.023(5) -0.021(4) -0.019(4) C15 0.053(4) 0.071(5) 0.046(4) 0.008(4) 0.001(3) -0.004(3) C16 0.066(5) 0.083(7) 0.082(6) -0.020(5) 0.022(4) -0.008(4) C17 0.144(10) 0.131(11) 0.079(7) 0.027(7) 0.034(6) -0.053(8) C18 0.095(7) 0.075(7) 0.082(7) 0.027(5) 0.003(5) 0.016(5) C19 0.057(4) 0.035(4) 0.048(4) 0.003(3) -0.015(3) 0.005(3) C20 0.079(5) 0.044(4) 0.052(5) 0.014(4) -0.020(3) -0.007(3) C21 0.097(6) 0.053(5) 0.080(6) 0.026(5) -0.033(5) -0.007(4) C22 0.104(7) 0.042(5) 0.083(7) 0.005(4) -0.039(5) 0.017(4) C23 0.068(5) 0.063(5) 0.076(6) -0.014(4) -0.023(4) 0.022(4) C24 0.072(5) 0.049(4) 0.052(5) 0.000(4) -0.013(3) 0.012(3) C25 0.142(10) 0.076(7) 0.146(11) 0.030(8) -0.063(8) 0.028(7) C26 0.072(5) 0.080(6) 0.080(6) 0.039(5) -0.011(4) -0.019(4) C27 0.065(5) 0.091(7) 0.095(7) 0.012(6) 0.008(4) 0.026(4) C28 0.049(5) 0.190(12) 0.115(9) 0.074(9) -0.041(5) -0.029(6) C29 0.071(6) 0.230(17) 0.101(9) 0.070(10) -0.017(6) 0.018(8) C30 0.112(9) 0.148(12) 0.109(9) 0.056(9) -0.051(7) -0.010(8) C31 0.078(5) 0.074(6) 0.053(5) 0.012(4) -0.007(4) -0.011(4) C32 0.081(5) 0.041(4) 0.081(6) -0.011(4) -0.011(4) 0.009(4) C33 0.126(9) 0.094(9) 0.110(10) -0.017(7) -0.009(7) 0.037(7) C34 0.223(15) 0.106(10) 0.076(9) -0.011(7) 0.027(9) 0.064(10) C35 0.186(12) 0.082(7) 0.067(7) -0.037(6) -0.035(6) 0.056(7) C36 0.054(4) 0.083(6) 0.065(5) -0.016(4) 0.008(3) -0.008(4) C37 0.086(7) 0.117(10) 0.133(11) 0.007(8) 0.041(7) -0.033(7) C38 0.086(7) 0.079(8) 0.217(15) 0.017(9) 0.058(8) -0.021(6) C39 0.092(7) 0.067(7) 0.182(13) -0.016(7) 0.050(7) -0.032(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 N1 2.467(5) . ? Ca1 O3 2.476(4) . ? Ca1 N3 2.487(5) . ? Ca1 O1 2.513(4) . ? Ca1 N2 2.541(6) . ? Ca1 O2 2.553(5) . ? Ca1 Ca2 3.4054(13) . ? Ca2 N2 2.528(5) 2_655 ? Ca2 N2 2.528(5) . ? Ca2 N3 2.580(5) 2_655 ? Ca2 N3 2.580(5) . ? Ca2 N1 2.610(6) 2_655 ? Ca2 N1 2.610(6) . ? Ca2 Ca1 3.4054(13) 2_655 ? O1 C28 1.414(9) . ? O1 C31 1.458(8) . ? O2 C35 1.447(11) . ? O2 C32 1.459(9) . ? O3 C39 1.452(11) . ? O3 C36 1.461(9) . ? N1 C1 1.406(9) . ? N1 H1A 0.9300 . ? N2 C10 1.401(7) . ? N2 H2A 0.9300 . ? N3 C19 1.408(7) . ? N3 H3B 0.9300 . ? C1 C2 1.427(9) . ? C1 C6 1.431(10) . ? C2 C3 1.427(11) . ? C2 C7 1.510(11) . ? C3 C4 1.371(12) . ? C3 H3A 0.9500 . ? C4 C5 1.378(12) . ? C4 C8 1.581(12) . ? C5 C6 1.423(11) . ? C5 H5A 0.9500 . ? C6 C9 1.495(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.424(10) . ? C10 C11 1.465(10) . ? C11 C12 1.389(9) . ? C11 C16 1.500(12) . ? C12 C13 1.395(14) . ? C12 H12A 0.9500 . ? C13 C14 1.409(14) . ? C13 C17 1.530(11) . ? C14 C15 1.404(10) . ? C14 H14A 0.9500 . ? C15 C18 1.499(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.421(9) . ? C19 C24 1.424(10) . ? C20 C21 1.409(10) . ? C20 C26 1.510(11) . ? C21 C22 1.367(13) . ? C21 H21A 0.9500 . ? C22 C23 1.376(11) . ? C22 C25 1.515(11) . ? C23 C24 1.398(10) . ? C23 H23A 0.9500 . ? C24 C27 1.485(11) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.441(12) . ? C28 H28A 0.9500 . ? C29 C30 1.462(14) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.468(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.508(14) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.519(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.477(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.458(13) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.543(18) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.411(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ca1 O3 135.35(17) . . ? N1 Ca1 N3 82.15(17) . . ? O3 Ca1 N3 136.03(19) . . ? N1 Ca1 O1 136.78(17) . . ? O3 Ca1 O1 79.52(16) . . ? N3 Ca1 O1 83.80(17) . . ? N1 Ca1 N2 81.08(17) . . ? O3 Ca1 N2 83.92(17) . . ? N3 Ca1 N2 80.52(17) . . ? O1 Ca1 N2 136.04(18) . . ? N1 Ca1 O2 83.79(18) . . ? O3 Ca1 O2 79.60(17) . . ? N3 Ca1 O2 136.01(18) . . ? O1 Ca1 O2 78.59(17) . . ? N2 Ca1 O2 137.57(17) . . ? N1 Ca1 Ca2 49.68(14) . . ? O3 Ca1 Ca2 131.56(13) . . ? N3 Ca1 Ca2 48.93(12) . . ? O1 Ca1 Ca2 132.72(13) . . ? N2 Ca1 Ca2 47.64(11) . . ? O2 Ca1 Ca2 133.46(11) . . ? N2 Ca2 N2 180.0(2) 2_655 . ? N2 Ca2 N3 79.02(15) 2_655 2_655 ? N2 Ca2 N3 100.98(15) . 2_655 ? N2 Ca2 N3 100.98(15) 2_655 . ? N2 Ca2 N3 79.02(15) . . ? N3 Ca2 N3 180.0(2) 2_655 . ? N2 Ca2 N1 78.62(17) 2_655 2_655 ? N2 Ca2 N1 101.38(17) . 2_655 ? N3 Ca2 N1 77.72(17) 2_655 2_655 ? N3 Ca2 N1 102.28(17) . 2_655 ? N2 Ca2 N1 101.38(17) 2_655 . ? N2 Ca2 N1 78.62(17) . . ? N3 Ca2 N1 102.28(17) 2_655 . ? N3 Ca2 N1 77.72(17) . . ? N1 Ca2 N1 180.0(3) 2_655 . ? N2 Ca2 Ca1 47.94(13) 2_655 2_655 ? N2 Ca2 Ca1 132.06(13) . 2_655 ? N3 Ca2 Ca1 46.64(11) 2_655 2_655 ? N3 Ca2 Ca1 133.36(11) . 2_655 ? N1 Ca2 Ca1 46.13(11) 2_655 2_655 ? N1 Ca2 Ca1 133.87(11) . 2_655 ? N2 Ca2 Ca1 132.06(13) 2_655 . ? N2 Ca2 Ca1 47.94(13) . . ? N3 Ca2 Ca1 133.36(11) 2_655 . ? N3 Ca2 Ca1 46.64(11) . . ? N1 Ca2 Ca1 133.87(11) 2_655 . ? N1 Ca2 Ca1 46.13(11) . . ? Ca1 Ca2 Ca1 180.00(5) 2_655 . ? C28 O1 C31 106.1(5) . . ? C28 O1 Ca1 125.5(5) . . ? C31 O1 Ca1 127.9(4) . . ? C35 O2 C32 107.7(6) . . ? C35 O2 Ca1 125.8(5) . . ? C32 O2 Ca1 126.1(4) . . ? C39 O3 C36 108.0(6) . . ? C39 O3 Ca1 125.0(5) . . ? C36 O3 Ca1 126.4(5) . . ? C1 N1 Ca1 129.4(5) . . ? C1 N1 Ca2 139.3(4) . . ? Ca1 N1 Ca2 84.20(16) . . ? C1 N1 H1A 98.3 . . ? Ca1 N1 H1A 98.3 . . ? Ca2 N1 H1A 98.3 . . ? C10 N2 Ca2 137.8(4) . . ? C10 N2 Ca1 131.1(4) . . ? Ca2 N2 Ca1 84.42(14) . . ? C10 N2 H2A 98.1 . . ? Ca2 N2 H2A 98.1 . . ? Ca1 N2 H2A 98.1 . . ? C19 N3 Ca1 131.4(4) . . ? C19 N3 Ca2 137.4(4) . . ? Ca1 N3 Ca2 84.43(14) . . ? C19 N3 H3B 98.1 . . ? Ca1 N3 H3B 98.1 . . ? Ca2 N3 H3B 98.1 . . ? N1 C1 C2 121.8(6) . . ? N1 C1 C6 122.0(6) . . ? C2 C1 C6 116.2(6) . . ? C3 C2 C1 119.0(7) . . ? C3 C2 C7 119.3(7) . . ? C1 C2 C7 121.7(6) . . ? C4 C3 C2 124.2(8) . . ? C4 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C3 C4 C5 117.5(7) . . ? C3 C4 C8 123.2(9) . . ? C5 C4 C8 119.3(9) . . ? C4 C5 C6 121.2(8) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 121.7(7) . . ? C5 C6 C9 119.0(7) . . ? C1 C6 C9 119.2(6) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C15 120.0(6) . . ? N2 C10 C11 122.9(6) . . ? C15 C10 C11 117.1(6) . . ? C12 C11 C10 120.5(8) . . ? C12 C11 C16 118.6(8) . . ? C10 C11 C16 120.9(6) . . ? C11 C12 C13 122.1(9) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C12 C13 C14 117.7(7) . . ? C12 C13 C17 122.1(9) . . ? C14 C13 C17 120.2(10) . . ? C15 C14 C13 122.8(8) . . ? C15 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? C14 C15 C10 119.7(7) . . ? C14 C15 C18 119.5(7) . . ? C10 C15 C18 120.7(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 123.1(6) . . ? N3 C19 C24 120.5(5) . . ? C20 C19 C24 116.4(6) . . ? C21 C20 C19 119.9(8) . . ? C21 C20 C26 119.2(6) . . ? C19 C20 C26 121.0(6) . . ? C22 C21 C20 123.9(7) . . ? C22 C21 H21A 118.1 . . ? C20 C21 H21A 118.1 . . ? C21 C22 C23 115.9(7) . . ? C21 C22 C25 121.6(9) . . ? C23 C22 C25 122.5(9) . . ? C22 C23 C24 124.0(8) . . ? C22 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C23 C24 C19 119.9(6) . . ? C23 C24 C27 120.9(7) . . ? C19 C24 C27 119.1(6) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 C29 109.9(8) . . ? O1 C28 H28A 125.1 . . ? C29 C28 H28A 125.1 . . ? C28 C29 C30 106.9(8) . . ? C28 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? C28 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C29 C30 C31 105.2(8) . . ? C29 C30 H30A 110.7 . . ? C31 C30 H30A 110.7 . . ? C29 C30 H30B 110.7 . . ? C31 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? O1 C31 C30 106.8(7) . . ? O1 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? O1 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? O2 C32 C33 105.9(7) . . ? O2 C32 H32A 110.6 . . ? C33 C32 H32A 110.6 . . ? O2 C32 H32B 110.6 . . ? C33 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? C32 C33 C34 106.0(9) . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? C32 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C35 C34 C33 105.1(11) . . ? C35 C34 H34A 110.7 . . ? C33 C34 H34A 110.7 . . ? C35 C34 H34B 110.7 . . ? C33 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? O2 C35 C34 109.9(9) . . ? O2 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? O2 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C37 C36 O3 106.5(8) . . ? C37 C36 H36A 110.4 . . ? O3 C36 H36A 110.4 . . ? C37 C36 H36B 110.4 . . ? O3 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C36 C37 C38 104.3(8) . . ? C36 C37 H37A 110.9 . . ? C38 C37 H37A 110.9 . . ? C36 C37 H37B 110.9 . . ? C38 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? C39 C38 C37 107.6(8) . . ? C39 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? C39 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? C38 C39 O3 108.5(9) . . ? C38 C39 H39A 110.0 . . ? O3 C39 H39A 110.0 . . ? C38 C39 H39B 110.0 . . ? O3 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.525 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.610 _refine_diff_density_max 0.361 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.071 #==== END data_FO3198 _database_code_depnum_ccdc_archive 'CCDC 666450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 Ca2 F8 N4 O7' _chemical_formula_weight 1097.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8241(3) _cell_length_b 22.4714(5) _cell_length_c 23.2769(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.4580(10) _cell_angle_gamma 90.00 _cell_volume 5548.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9504 _exptl_absorpt_correction_T_max 0.9706 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37280 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12664 _reflns_number_gt 7533 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+3.9466P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12664 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.65521(5) 0.16687(2) 0.75183(3) 0.03067(15) Uani 1 1 d . . . Ca2 Ca 0.44125(5) 0.06887(2) 0.68788(2) 0.02777(14) Uani 1 1 d . . . F1 F 0.4067(2) 0.22438(9) 0.62410(9) 0.0585(5) Uani 1 1 d . . . F2 F 0.2866(2) 0.22348(9) 0.80726(9) 0.0605(6) Uani 1 1 d . . . F3 F 0.79434(16) 0.04254(8) 0.69474(8) 0.0437(4) Uani 1 1 d . . . F4 F 0.59750(17) 0.16185(8) 0.53678(8) 0.0473(5) Uani 1 1 d . . . F5 F 0.76271(18) -0.02934(8) 0.82512(9) 0.0517(5) Uani 1 1 d . . . F6 F 0.41799(17) 0.09397(8) 0.83828(8) 0.0475(5) Uani 1 1 d . . . F7 F 0.25051(18) -0.03189(10) 0.61242(8) 0.0559(5) Uani 1 1 d . . . F8 F 0.1400(2) -0.03603(10) 0.79738(9) 0.0714(7) Uani 1 1 d . . . O1 O 0.6879(3) 0.26466(10) 0.71623(11) 0.0580(7) Uani 1 1 d . . . O2 O 0.6929(2) 0.21416(11) 0.84617(10) 0.0533(6) Uani 1 1 d . . . O3 O 0.8763(2) 0.15123(11) 0.77764(11) 0.0516(6) Uani 1 1 d . B . O4 O 0.53319(19) -0.01647(9) 0.64910(9) 0.0381(5) Uani 1 1 d . . . O5 O 0.2892(2) 0.09921(11) 0.60497(10) 0.0551(6) Uani 1 1 d . . . N1 N 0.4258(2) 0.17027(11) 0.73270(12) 0.0343(6) Uani 1 1 d . . . H1N1 H 0.414(3) 0.1604(13) 0.7641(14) 0.030(9) Uiso 1 1 d . . . N2 N 0.6146(2) 0.12754(11) 0.65352(10) 0.0303(5) Uani 1 1 d . . . H1N2 H 0.570(3) 0.1542(14) 0.6339(14) 0.036(9) Uiso 1 1 d . . . N3 N 0.6084(2) 0.06533(11) 0.77841(10) 0.0312(5) Uani 1 1 d . . . H1N3 H 0.668(3) 0.0481(14) 0.7669(14) 0.040(9) Uiso 1 1 d . . . N4 N 0.2961(2) 0.00992(11) 0.72574(12) 0.0378(6) Uani 1 1 d . . . H1N4 H 0.296(4) 0.0168(18) 0.7622(18) 0.068(13) Uiso 1 1 d . . . C1 C 0.3511(2) 0.21882(12) 0.71687(13) 0.0322(6) Uani 1 1 d . . . C2 C 0.3382(3) 0.24717(13) 0.66243(14) 0.0387(7) Uani 1 1 d . . . C3 C 0.2639(3) 0.29557(15) 0.64450(17) 0.0516(9) Uani 1 1 d . . . H3A H 0.2598 0.3119 0.6065 0.062 Uiso 1 1 calc R . . C4 C 0.1953(4) 0.32017(17) 0.6822(2) 0.0664(11) Uani 1 1 d . . . H4A H 0.1433 0.3539 0.6706 0.080 Uiso 1 1 calc R . . C5 C 0.2027(4) 0.29545(17) 0.73694(19) 0.0640(11) Uani 1 1 d . . . H5A H 0.1557 0.3118 0.7636 0.077 Uiso 1 1 calc R . . C6 C 0.2787(3) 0.24691(14) 0.75244(15) 0.0433(8) Uani 1 1 d . . . C7 C 0.6887(2) 0.10364(12) 0.61809(12) 0.0283(6) Uani 1 1 d . . . C8 C 0.7796(3) 0.05941(13) 0.63733(13) 0.0332(6) Uani 1 1 d . . . C9 C 0.8527(3) 0.03229(14) 0.60318(16) 0.0430(8) Uani 1 1 d . . . H9A H 0.9126 0.0028 0.6193 0.052 Uiso 1 1 calc R . . C10 C 0.8377(3) 0.04856(15) 0.54480(16) 0.0494(9) Uani 1 1 d . . . H10A H 0.8862 0.0297 0.5202 0.059 Uiso 1 1 calc R . . C11 C 0.7520(3) 0.09240(15) 0.52252(15) 0.0458(8) Uani 1 1 d . . . H11A H 0.7411 0.1042 0.4827 0.055 Uiso 1 1 calc R . . C12 C 0.6833(3) 0.11839(13) 0.55903(13) 0.0347(7) Uani 1 1 d . . . C13 C 0.5919(3) 0.03484(12) 0.82765(12) 0.0316(6) Uani 1 1 d . . . C14 C 0.6659(3) -0.01353(13) 0.85245(13) 0.0384(7) Uani 1 1 d . . . C15 C 0.6500(4) -0.04510(15) 0.90113(15) 0.0506(9) Uani 1 1 d . . . H15A H 0.7045 -0.0773 0.9153 0.061 Uiso 1 1 calc R . . C16 C 0.5537(4) -0.02930(16) 0.92893(15) 0.0544(9) Uani 1 1 d . . . H16A H 0.5406 -0.0507 0.9624 0.065 Uiso 1 1 calc R . . C17 C 0.4763(3) 0.01807(16) 0.90750(14) 0.0473(8) Uani 1 1 d . . . H17A H 0.4099 0.0298 0.9263 0.057 Uiso 1 1 calc R . . C18 C 0.4968(3) 0.04778(13) 0.85876(13) 0.0365(7) Uani 1 1 d . . . C19 C 0.2030(3) -0.02974(12) 0.70684(13) 0.0324(6) Uani 1 1 d . . . C20 C 0.1763(3) -0.05239(13) 0.64937(13) 0.0356(7) Uani 1 1 d . . . C21 C 0.0839(3) -0.09284(14) 0.62791(15) 0.0444(8) Uani 1 1 d . . . H21A H 0.0729 -0.1061 0.5885 0.053 Uiso 1 1 calc R . . C22 C 0.0074(4) -0.11418(16) 0.66369(19) 0.0583(10) Uani 1 1 d . . . H22A H -0.0573 -0.1422 0.6495 0.070 Uiso 1 1 calc R . . C23 C 0.0267(4) -0.09399(17) 0.72088(19) 0.0627(11) Uani 1 1 d . . . H23A H -0.0253 -0.1078 0.7465 0.075 Uiso 1 1 calc R . . C24 C 0.1209(3) -0.05404(15) 0.74035(15) 0.0464(8) Uani 1 1 d . . . C25 C 0.7363(6) 0.2786(2) 0.6652(3) 0.1016(18) Uani 1 1 d . . . H25A H 0.7138 0.2469 0.6354 0.122 Uiso 1 1 calc R . . H25B H 0.8293 0.2819 0.6752 0.122 Uiso 1 1 calc R . . C26 C 0.6814(9) 0.3347(3) 0.6424(3) 0.145(3) Uani 1 1 d . . . H26A H 0.6285 0.3287 0.6029 0.174 Uiso 1 1 calc R . . H26B H 0.7488 0.3635 0.6390 0.174 Uiso 1 1 calc R . . C27 C 0.6040(5) 0.3577(2) 0.6828(3) 0.099(2) Uani 1 1 d . . . H27A H 0.5130 0.3542 0.6655 0.119 Uiso 1 1 calc R . . H27B H 0.6241 0.3999 0.6926 0.119 Uiso 1 1 calc R . . C28 C 0.6387(4) 0.31929(16) 0.7355(2) 0.0745(13) Uani 1 1 d . . . H28A H 0.7033 0.3391 0.7655 0.089 Uiso 1 1 calc R . . H28B H 0.5638 0.3111 0.7527 0.089 Uiso 1 1 calc R . . C29 C 0.7970(5) 0.2525(2) 0.8706(2) 0.0923(17) Uani 1 1 d . . . H29A H 0.8766 0.2358 0.8627 0.111 Uiso 1 1 calc R . . H29B H 0.7845 0.2924 0.8523 0.111 Uiso 1 1 calc R . . C30 C 0.8039(5) 0.2572(3) 0.9304(2) 0.0978(18) Uani 1 1 d . . . H30A H 0.8222 0.2988 0.9433 0.117 Uiso 1 1 calc R . . H30B H 0.8721 0.2315 0.9517 0.117 Uiso 1 1 calc R . . C31 C 0.6804(4) 0.2383(2) 0.94308(18) 0.0741(12) Uani 1 1 d . . . H31A H 0.6272 0.2731 0.9475 0.089 Uiso 1 1 calc R . . H31B H 0.6920 0.2139 0.9792 0.089 Uiso 1 1 calc R . . C32 C 0.6229(4) 0.2020(2) 0.89020(17) 0.0692(12) Uani 1 1 d . . . H32A H 0.6271 0.1591 0.9000 0.083 Uiso 1 1 calc R . . H32B H 0.5334 0.2132 0.8765 0.083 Uiso 1 1 calc R . . C33 C 0.9685(3) 0.15898(19) 0.7413(2) 0.0666(11) Uani 1 1 d . B . H33A H 1.0059 0.1993 0.7466 0.080 Uiso 1 1 calc R . . H33B H 0.9294 0.1535 0.6994 0.080 Uiso 1 1 calc R . . C34 C 1.0681(4) 0.1121(2) 0.7610(3) 0.0947(17) Uani 1 1 d . . . H34A H 1.0426 0.0737 0.7412 0.114 Uiso 0.50 1 calc PR A 1 H34B H 1.1496 0.1244 0.7516 0.114 Uiso 0.50 1 calc PR A 1 H34C H 1.1498 0.1297 0.7763 0.114 Uiso 0.50 1 d PR A 2 H34D H 1.0751 0.0850 0.7293 0.114 Uiso 0.50 1 d PR A 2 C35 C 1.0779(8) 0.1068(4) 0.8186(4) 0.060(2) Uiso 0.50 1 d P B 1 H35A H 1.1312 0.1387 0.8399 0.073 Uiso 0.50 1 calc PR B 1 H35B H 1.1133 0.0676 0.8327 0.073 Uiso 0.50 1 calc PR B 1 C35A C 1.0068(9) 0.0757(4) 0.8151(4) 0.069(2) Uiso 0.50 1 d P B 2 H35C H 0.9637 0.0382 0.8003 0.083 Uiso 0.50 1 calc PR B 2 H35D H 1.0731 0.0669 0.8499 0.083 Uiso 0.50 1 calc PR B 2 C36 C 0.9310(4) 0.1133(3) 0.8262(2) 0.0957(18) Uani 1 1 d . . . H36A H 0.8886 0.0741 0.8234 0.115 Uiso 0.50 1 calc PR B 1 H36B H 0.9260 0.1320 0.8642 0.115 Uiso 0.50 1 calc PR B 1 H34E H 0.9710 0.1379 0.8589 0.115 Uiso 0.50 1 d PR B 2 H34F H 0.8633 0.0916 0.8385 0.115 Uiso 0.50 1 d PR B 2 C37 C 0.5597(4) -0.06688(15) 0.68795(16) 0.0574(10) Uani 1 1 d . . . H37A H 0.5001 -0.0684 0.7151 0.069 Uiso 1 1 calc R . . H37B H 0.6467 -0.0647 0.7112 0.069 Uiso 1 1 calc R . . C38 C 0.5441(5) -0.11979(17) 0.64885(19) 0.0716(12) Uani 1 1 d . . . H38A H 0.4552 -0.1330 0.6396 0.086 Uiso 1 1 calc R . . H38B H 0.5977 -0.1532 0.6670 0.086 Uiso 1 1 calc R . . C39 C 0.5862(4) -0.09743(17) 0.59480(18) 0.0629(11) Uani 1 1 d . . . H39A H 0.6792 -0.0974 0.6001 0.076 Uiso 1 1 calc R . . H39B H 0.5500 -0.1216 0.5600 0.076 Uiso 1 1 calc R . . C40 C 0.5341(3) -0.03521(14) 0.58971(14) 0.0419(7) Uani 1 1 d . . . H40A H 0.5881 -0.0086 0.5714 0.050 Uiso 1 1 calc R . . H40B H 0.4478 -0.0347 0.5656 0.050 Uiso 1 1 calc R . . C41 C 0.1651(3) 0.11703(19) 0.61231(19) 0.0629(11) Uani 1 1 d . . . H41A H 0.1703 0.1434 0.6468 0.076 Uiso 1 1 calc R . . H41B H 0.1130 0.0819 0.6173 0.076 Uiso 1 1 calc R . . C42 C 0.1110(4) 0.14990(18) 0.55608(19) 0.0665(12) Uani 1 1 d . . . H42A H 0.0177 0.1485 0.5475 0.080 Uiso 1 1 calc R . . H42B H 0.1388 0.1920 0.5582 0.080 Uiso 1 1 calc R . . C43 C 0.1641(4) 0.11619(19) 0.51106(19) 0.0738(13) Uani 1 1 d . . . H43A H 0.1683 0.1415 0.4767 0.089 Uiso 1 1 calc R . . H43B H 0.1131 0.0804 0.4978 0.089 Uiso 1 1 calc R . . C44 C 0.2944(4) 0.09937(19) 0.54350(16) 0.0617(10) Uani 1 1 d . . . H44A H 0.3180 0.0595 0.5311 0.074 Uiso 1 1 calc R . . H44B H 0.3573 0.1286 0.5356 0.074 Uiso 1 1 calc R . . O1TA O 0.655(3) -0.2485(16) 1.0314(15) 0.388(15) Uiso 0.50 1 d P C 1 C1TA C 0.8114(14) -0.2210(7) 1.0587(6) 0.068(4) Uiso 0.50 1 d P C 1 H1TA H 0.8422 -0.2322 1.1002 0.082 Uiso 0.50 1 calc PR C 1 H1TB H 0.8715 -0.2354 1.0349 0.082 Uiso 0.50 1 calc PR C 1 C2TA C 0.7893(8) -0.1519(4) 1.0517(4) 0.062(2) Uiso 0.50 1 d P C 1 H2TA H 0.7680 -0.1359 1.0881 0.075 Uiso 0.50 1 calc PR C 1 H2TB H 0.8685 -0.1327 1.0463 0.075 Uiso 0.50 1 calc PR C 1 C3TA C 0.7018(8) -0.1385(4) 1.0087(4) 0.0500(19) Uiso 0.50 1 d P C 1 H3TA H 0.7348 -0.1371 0.9720 0.060 Uiso 0.50 1 calc PR C 1 H3TB H 0.6663 -0.0990 1.0150 0.060 Uiso 0.50 1 calc PR C 1 C4TA C 0.6068(11) -0.1835(5) 1.0050(6) 0.071(3) Uiso 0.50 1 d P C 1 H4TA H 0.5663 -0.1885 0.9632 0.086 Uiso 0.50 1 calc PR C 1 H4TB H 0.5414 -0.1690 1.0258 0.086 Uiso 0.50 1 calc PR C 1 O1TC O 0.6702(7) -0.2391(3) 1.0377(3) 0.076 Uiso 0.50 1 d P D 2 C1TC C 0.807(2) -0.2349(9) 1.0616(9) 0.119(8) Uiso 0.50 1 d P D 2 H1TC H 0.8231 -0.2317 1.1049 0.143 Uiso 0.50 1 calc PR D 2 H1TD H 0.8512 -0.2703 1.0506 0.143 Uiso 0.50 1 calc PR D 2 C2TC C 0.8455(12) -0.1831(6) 1.0364(6) 0.114(4) Uiso 0.50 1 d P D 2 H2TC H 0.9072 -0.1932 1.0117 0.137 Uiso 0.50 1 calc PR D 2 H2TD H 0.8860 -0.1553 1.0675 0.137 Uiso 0.50 1 calc PR D 2 C3TC C 0.7371(8) -0.1564(4) 1.0017(4) 0.060(2) Uiso 0.50 1 d P D 2 H3TC H 0.7441 -0.1125 1.0042 0.072 Uiso 0.50 1 calc PR D 2 H3TD H 0.7291 -0.1683 0.9602 0.072 Uiso 0.50 1 calc PR D 2 C4TC C 0.6324(15) -0.1755(7) 1.0230(7) 0.110(6) Uiso 0.50 1 d P D 2 H4TC H 0.5541 -0.1730 0.9928 0.132 Uiso 0.50 1 calc PR D 2 H4TD H 0.6218 -0.1528 1.0582 0.132 Uiso 0.50 1 calc PR D 2 O1TB O 0.0904(6) -0.1128(3) 1.0128(3) 0.0780(17) Uiso 0.50 1 d P E 1 C1TB C 0.0088(14) -0.1044(6) 0.9555(6) 0.112(4) Uiso 0.50 1 d P E 1 H1TE H -0.0804 -0.1074 0.9594 0.135 Uiso 0.50 1 calc PR E 1 H1TF H 0.0251 -0.1363 0.9287 0.135 Uiso 0.50 1 calc PR E 1 C2TB C 0.0313(10) -0.0432(5) 0.9289(5) 0.082(3) Uiso 0.50 1 d P E 1 H2TE H 0.0272 -0.0466 0.8862 0.098 Uiso 0.50 1 calc PR E 1 H2TF H -0.0324 -0.0139 0.9359 0.098 Uiso 0.50 1 calc PR E 1 C3TB C 0.1543(19) -0.0261(9) 0.9584(9) 0.104(6) Uiso 0.50 1 d P E 1 H3TE H 0.1572 0.0164 0.9700 0.125 Uiso 0.50 1 calc PR E 1 H3TF H 0.2179 -0.0335 0.9339 0.125 Uiso 0.50 1 calc PR E 1 C4TB C 0.1753(11) -0.0706(5) 1.0164(5) 0.088(3) Uiso 0.50 1 d P E 1 H4TE H 0.2597 -0.0892 1.0213 0.106 Uiso 0.50 1 calc PR E 1 H4TF H 0.1736 -0.0464 1.0517 0.106 Uiso 0.50 1 calc PR E 1 O1TD O 0.1436(11) -0.1290(5) 0.9887(5) 0.152(4) Uiso 0.50 1 d P F 2 C1TD C 0.0508(14) -0.1286(6) 0.9440(6) 0.109(4) Uiso 0.50 1 d P F 2 H1TG H -0.0283 -0.1408 0.9559 0.130 Uiso 0.50 1 calc PR F 2 H1TH H 0.0677 -0.1563 0.9134 0.130 Uiso 0.50 1 calc PR F 2 C2TD C 0.0412(10) -0.0732(5) 0.9238(5) 0.075(3) Uiso 0.50 1 d P F 2 H2TG H -0.0341 -0.0535 0.9334 0.090 Uiso 0.50 1 calc PR F 2 H2TH H 0.0335 -0.0729 0.8807 0.090 Uiso 0.50 1 calc PR F 2 C3TD C 0.1641(16) -0.0400(7) 0.9543(8) 0.083(5) Uiso 0.50 1 d P F 2 H3TG H 0.2196 -0.0324 0.9260 0.099 Uiso 0.50 1 calc PR F 2 H3TH H 0.1434 -0.0015 0.9708 0.099 Uiso 0.50 1 calc PR F 2 C4TD C 0.2178(9) -0.0755(4) 0.9954(5) 0.071(3) Uiso 0.50 1 d P F 2 H4TG H 0.2197 -0.0575 1.0344 0.086 Uiso 0.50 1 calc PR F 2 H4TH H 0.3054 -0.0842 0.9914 0.086 Uiso 0.50 1 calc PR F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0296(3) 0.0315(3) 0.0320(3) -0.0048(2) 0.0088(2) -0.0027(2) Ca2 0.0254(3) 0.0304(3) 0.0280(3) -0.0003(2) 0.0063(2) -0.0004(2) F1 0.0712(13) 0.0586(12) 0.0522(12) 0.0178(10) 0.0279(10) 0.0248(11) F2 0.0709(14) 0.0645(13) 0.0525(12) -0.0037(10) 0.0277(10) 0.0222(11) F3 0.0396(10) 0.0495(10) 0.0418(10) 0.0062(8) 0.0082(8) 0.0095(8) F4 0.0538(11) 0.0515(11) 0.0381(10) 0.0118(9) 0.0130(9) 0.0037(9) F5 0.0523(11) 0.0487(11) 0.0526(12) 0.0051(9) 0.0065(9) 0.0137(9) F6 0.0457(10) 0.0578(11) 0.0433(10) 0.0070(9) 0.0189(8) 0.0078(9) F7 0.0472(11) 0.0845(15) 0.0401(11) -0.0099(10) 0.0183(9) -0.0134(10) F8 0.0929(17) 0.0820(15) 0.0498(13) -0.0100(11) 0.0399(12) -0.0331(13) O1 0.0807(18) 0.0335(12) 0.0642(16) 0.0009(11) 0.0251(14) -0.0060(12) O2 0.0537(14) 0.0634(15) 0.0453(14) -0.0225(12) 0.0158(11) -0.0191(12) O3 0.0313(12) 0.0644(15) 0.0602(15) -0.0087(13) 0.0113(11) -0.0027(11) O4 0.0422(12) 0.0346(11) 0.0378(12) -0.0073(9) 0.0091(9) 0.0018(9) O5 0.0365(12) 0.0747(17) 0.0484(14) 0.0221(13) -0.0054(10) -0.0044(11) N1 0.0345(13) 0.0350(13) 0.0357(15) 0.0007(12) 0.0127(12) 0.0061(11) N2 0.0315(13) 0.0315(12) 0.0298(13) 0.0010(11) 0.0105(10) 0.0052(11) N3 0.0300(12) 0.0341(13) 0.0304(13) 0.0032(11) 0.0080(10) 0.0019(11) N4 0.0394(14) 0.0400(14) 0.0363(15) -0.0041(12) 0.0135(12) -0.0082(11) C1 0.0254(14) 0.0262(14) 0.0444(17) -0.0051(13) 0.0059(12) 0.0008(11) C2 0.0375(16) 0.0340(16) 0.0458(18) -0.0015(14) 0.0114(14) 0.0040(13) C3 0.051(2) 0.0391(18) 0.063(2) 0.0092(17) 0.0066(17) 0.0088(16) C4 0.068(3) 0.049(2) 0.082(3) 0.008(2) 0.013(2) 0.0320(19) C5 0.065(2) 0.053(2) 0.078(3) -0.005(2) 0.023(2) 0.0293(19) C6 0.0461(18) 0.0403(17) 0.0456(19) -0.0062(15) 0.0142(15) 0.0070(15) C7 0.0273(14) 0.0287(14) 0.0299(15) -0.0047(12) 0.0083(11) -0.0063(11) C8 0.0292(14) 0.0345(15) 0.0375(16) -0.0040(13) 0.0101(12) -0.0032(12) C9 0.0309(16) 0.0399(17) 0.062(2) -0.0094(16) 0.0191(15) 0.0002(13) C10 0.049(2) 0.051(2) 0.058(2) -0.0224(17) 0.0341(17) -0.0104(16) C11 0.053(2) 0.054(2) 0.0362(17) -0.0102(15) 0.0231(15) -0.0157(17) C12 0.0348(16) 0.0347(15) 0.0362(16) -0.0029(13) 0.0113(13) -0.0100(13) C13 0.0341(15) 0.0341(15) 0.0248(14) -0.0011(12) 0.0013(12) -0.0087(12) C14 0.0454(18) 0.0367(16) 0.0304(16) -0.0012(13) 0.0010(13) -0.0035(14) C15 0.070(2) 0.0384(18) 0.0384(19) 0.0071(15) -0.0022(17) -0.0038(17) C16 0.080(3) 0.052(2) 0.0310(18) 0.0083(16) 0.0116(18) -0.0144(19) C17 0.058(2) 0.056(2) 0.0302(16) 0.0004(15) 0.0141(15) -0.0117(17) C18 0.0414(17) 0.0392(16) 0.0288(15) 0.0019(13) 0.0066(13) -0.0042(14) C19 0.0322(15) 0.0288(14) 0.0385(16) 0.0017(13) 0.0128(12) 0.0024(12) C20 0.0299(15) 0.0374(16) 0.0412(17) -0.0010(14) 0.0113(13) 0.0045(12) C21 0.0378(17) 0.0403(17) 0.050(2) -0.0062(15) -0.0025(15) 0.0036(14) C22 0.053(2) 0.0430(19) 0.076(3) -0.0029(19) 0.007(2) -0.0143(17) C23 0.059(2) 0.057(2) 0.077(3) 0.006(2) 0.027(2) -0.0245(19) C24 0.054(2) 0.0444(18) 0.0450(19) -0.0010(15) 0.0190(16) -0.0106(16) C25 0.145(5) 0.068(3) 0.113(4) 0.021(3) 0.075(4) -0.013(3) C26 0.239(9) 0.103(5) 0.095(5) 0.048(4) 0.042(5) 0.027(5) C27 0.085(3) 0.045(2) 0.149(5) 0.017(3) -0.023(4) -0.002(2) C28 0.084(3) 0.0355(19) 0.108(4) -0.015(2) 0.028(3) -0.007(2) C29 0.086(3) 0.117(4) 0.077(3) -0.049(3) 0.023(3) -0.057(3) C30 0.100(4) 0.125(4) 0.068(3) -0.043(3) 0.016(3) -0.052(3) C31 0.089(3) 0.085(3) 0.051(2) -0.024(2) 0.020(2) -0.012(3) C32 0.074(3) 0.085(3) 0.053(2) -0.025(2) 0.024(2) -0.024(2) C33 0.043(2) 0.072(3) 0.091(3) -0.015(2) 0.026(2) -0.0093(19) C34 0.043(2) 0.095(4) 0.146(5) -0.033(3) 0.019(3) 0.017(2) C36 0.058(3) 0.126(4) 0.087(4) 0.031(3) -0.026(3) -0.016(3) C37 0.081(3) 0.0402(19) 0.051(2) -0.0004(17) 0.0117(19) 0.0099(18) C38 0.101(3) 0.041(2) 0.069(3) -0.0028(19) 0.006(2) 0.008(2) C39 0.076(3) 0.053(2) 0.061(2) -0.0204(19) 0.014(2) 0.008(2) C40 0.0423(17) 0.0448(18) 0.0400(18) -0.0135(15) 0.0119(14) -0.0083(14) C41 0.0342(18) 0.073(3) 0.077(3) 0.015(2) 0.0004(18) -0.0066(17) C42 0.047(2) 0.059(2) 0.082(3) 0.014(2) -0.015(2) -0.0033(18) C43 0.081(3) 0.062(3) 0.061(3) 0.010(2) -0.030(2) -0.005(2) C44 0.060(2) 0.074(3) 0.044(2) 0.0110(19) -0.0036(18) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O3 2.375(2) . ? Ca1 O1 2.399(2) . ? Ca1 O2 2.400(2) . ? Ca1 N2 2.411(2) . ? Ca1 N1 2.436(3) . ? Ca1 N3 2.443(2) . ? Ca1 Ca2 3.3256(8) . ? Ca2 N4 2.356(3) . ? Ca2 O5 2.374(2) . ? Ca2 O4 2.417(2) . ? Ca2 N3 2.491(2) . ? Ca2 N1 2.526(3) . ? Ca2 N2 2.549(2) . ? F1 C2 1.367(4) . ? F2 C6 1.367(4) . ? F3 C8 1.368(3) . ? F4 C12 1.376(3) . ? F5 C14 1.376(4) . ? F6 C18 1.368(3) . ? F7 C20 1.368(3) . ? F8 C24 1.364(4) . ? O1 C25 1.426(5) . ? O1 C28 1.444(4) . ? O2 C32 1.417(4) . ? O2 C29 1.443(4) . ? O3 C33 1.442(4) . ? O3 C36 1.446(5) . ? O4 C37 1.442(4) . ? O4 C40 1.447(4) . ? O5 C41 1.444(4) . ? O5 C44 1.443(4) . ? N1 C1 1.364(4) . ? N2 C7 1.369(3) . ? N3 C13 1.377(4) . ? N4 C19 1.352(4) . ? C1 C6 1.398(4) . ? C1 C2 1.400(4) . ? C2 C3 1.368(4) . ? C3 C4 1.373(5) . ? C4 C5 1.379(6) . ? C5 C6 1.371(5) . ? C7 C12 1.404(4) . ? C7 C8 1.408(4) . ? C8 C9 1.371(4) . ? C9 C10 1.385(5) . ? C10 C11 1.382(5) . ? C11 C12 1.366(4) . ? C13 C18 1.401(4) . ? C13 C14 1.405(4) . ? C14 C15 1.376(4) . ? C15 C16 1.378(5) . ? C16 C17 1.385(5) . ? C17 C18 1.372(4) . ? C19 C24 1.404(4) . ? C19 C20 1.407(4) . ? C20 C21 1.370(4) . ? C21 C22 1.373(5) . ? C22 C23 1.382(6) . ? C23 C24 1.367(5) . ? C25 C26 1.448(8) . ? C26 C27 1.473(8) . ? C27 C28 1.486(7) . ? C29 C30 1.383(6) . ? C30 C31 1.487(6) . ? C31 C32 1.504(5) . ? C33 C34 1.512(6) . ? C34 C35 1.329(9) . ? C34 C35A 1.741(10) . ? C35 C36 1.640(9) . ? C35A C36 1.240(9) . ? C37 C38 1.487(5) . ? C38 C39 1.506(6) . ? C39 C40 1.503(5) . ? C41 C42 1.515(5) . ? C42 C43 1.497(6) . ? C43 C44 1.509(5) . ? O1TA C4TA 1.63(4) . ? O1TA C1TA 1.80(4) . ? C1TA C2TA 1.574(18) . ? C2TA C3TA 1.270(11) . ? C3TA C4TA 1.432(14) . ? O1TC C4TC 1.507(18) . ? O1TC C1TC 1.47(2) . ? C1TC C2TC 1.41(2) . ? C2TC C3TC 1.418(15) . ? C3TC C4TC 1.392(18) . ? O1TB C4TB 1.311(12) . ? O1TB C1TB 1.458(15) . ? C1TB C2TB 1.545(17) . ? C2TB C3TB 1.42(2) . ? C3TB C4TB 1.66(2) . ? O1TD C1TD 1.296(15) . ? O1TD C4TD 1.436(14) . ? C1TD C2TD 1.327(17) . ? C2TD C3TD 1.57(2) . ? C3TD C4TD 1.292(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ca1 O1 90.73(9) . . ? O3 Ca1 O2 81.64(8) . . ? O1 Ca1 O2 84.29(9) . . ? O3 Ca1 N2 99.81(8) . . ? O1 Ca1 N2 91.12(9) . . ? O2 Ca1 N2 175.22(9) . . ? O3 Ca1 N1 172.10(9) . . ? O1 Ca1 N1 97.07(9) . . ? O2 Ca1 N1 97.75(9) . . ? N2 Ca1 N1 81.44(9) . . ? O3 Ca1 N3 92.70(9) . . ? O1 Ca1 N3 174.21(9) . . ? O2 Ca1 N3 100.82(9) . . ? N2 Ca1 N3 83.70(8) . . ? N1 Ca1 N3 79.65(9) . . ? O3 Ca1 Ca2 126.33(6) . . ? O1 Ca1 Ca2 126.10(7) . . ? O2 Ca1 Ca2 132.78(6) . . ? N2 Ca1 Ca2 49.68(6) . . ? N1 Ca1 Ca2 49.07(6) . . ? N3 Ca1 Ca2 48.24(6) . . ? N4 Ca2 O5 93.41(9) . . ? N4 Ca2 O4 92.77(8) . . ? O5 Ca2 O4 101.23(9) . . ? N4 Ca2 N3 95.27(9) . . ? O5 Ca2 N3 165.14(9) . . ? O4 Ca2 N3 90.39(8) . . ? N4 Ca2 N1 104.41(9) . . ? O5 Ca2 N1 89.12(9) . . ? O4 Ca2 N1 159.45(8) . . ? N3 Ca2 N1 77.05(8) . . ? N4 Ca2 N2 174.62(9) . . ? O5 Ca2 N2 91.78(8) . . ? O4 Ca2 N2 84.82(7) . . ? N3 Ca2 N2 79.96(8) . . ? N1 Ca2 N2 77.08(8) . . ? N4 Ca2 Ca1 131.44(7) . . ? O5 Ca2 Ca1 118.84(6) . . ? O4 Ca2 Ca1 113.01(5) . . ? N3 Ca2 Ca1 47.03(6) . . ? N1 Ca2 Ca1 46.77(6) . . ? N2 Ca2 Ca1 46.14(5) . . ? C25 O1 C28 106.9(3) . . ? C25 O1 Ca1 126.3(2) . . ? C28 O1 Ca1 125.6(2) . . ? C32 O2 C29 108.5(3) . . ? C32 O2 Ca1 124.0(2) . . ? C29 O2 Ca1 127.0(2) . . ? C33 O3 C36 107.8(3) . . ? C33 O3 Ca1 127.9(2) . . ? C36 O3 Ca1 121.4(2) . . ? C37 O4 C40 109.4(2) . . ? C37 O4 Ca2 115.76(19) . . ? C40 O4 Ca2 132.01(18) . . ? C41 O5 C44 109.7(3) . . ? C41 O5 Ca2 119.6(2) . . ? C44 O5 Ca2 130.5(2) . . ? C1 N1 Ca1 127.04(19) . . ? C1 N1 Ca2 134.0(2) . . ? Ca1 N1 Ca2 84.16(8) . . ? C7 N2 Ca1 134.25(19) . . ? C7 N2 Ca2 122.81(18) . . ? Ca1 N2 Ca2 84.17(7) . . ? C13 N3 Ca1 138.00(19) . . ? C13 N3 Ca2 121.83(18) . . ? Ca1 N3 Ca2 84.74(7) . . ? C19 N4 Ca2 139.3(2) . . ? N1 C1 C6 124.9(3) . . ? N1 C1 C2 123.8(3) . . ? C6 C1 C2 111.3(3) . . ? F1 C2 C3 117.4(3) . . ? F1 C2 C1 116.8(2) . . ? C3 C2 C1 125.8(3) . . ? C2 C3 C4 119.0(4) . . ? C3 C4 C5 119.3(3) . . ? C6 C5 C4 119.0(4) . . ? F2 C6 C5 118.3(3) . . ? F2 C6 C1 116.1(3) . . ? C5 C6 C1 125.5(3) . . ? N2 C7 C12 125.6(3) . . ? N2 C7 C8 122.8(3) . . ? C12 C7 C8 111.6(3) . . ? F3 C8 C9 118.3(3) . . ? F3 C8 C7 116.4(2) . . ? C9 C8 C7 125.2(3) . . ? C8 C9 C10 118.9(3) . . ? C11 C10 C9 119.7(3) . . ? C12 C11 C10 118.6(3) . . ? C11 C12 F4 118.6(3) . . ? C11 C12 C7 125.9(3) . . ? F4 C12 C7 115.4(2) . . ? N3 C13 C18 123.8(3) . . ? N3 C13 C14 124.7(3) . . ? C18 C13 C14 111.4(3) . . ? F5 C14 C15 118.6(3) . . ? F5 C14 C13 115.7(3) . . ? C15 C14 C13 125.7(3) . . ? C16 C15 C14 118.9(3) . . ? C15 C16 C17 119.3(3) . . ? C18 C17 C16 119.1(3) . . ? F6 C18 C17 117.7(3) . . ? F6 C18 C13 116.7(2) . . ? C17 C18 C13 125.6(3) . . ? N4 C19 C24 126.1(3) . . ? N4 C19 C20 123.2(3) . . ? C24 C19 C20 110.8(3) . . ? C21 C20 F7 118.1(3) . . ? C21 C20 C19 125.7(3) . . ? F7 C20 C19 116.1(3) . . ? C20 C21 C22 119.7(3) . . ? C21 C22 C23 118.4(3) . . ? C24 C23 C22 119.7(3) . . ? F8 C24 C23 118.5(3) . . ? F8 C24 C19 115.8(3) . . ? C23 C24 C19 125.8(3) . . ? O1 C25 C26 107.7(5) . . ? C25 C26 C27 108.4(5) . . ? C26 C27 C28 103.9(4) . . ? O1 C28 C27 106.6(4) . . ? C30 C29 O2 108.9(4) . . ? C29 C30 C31 107.9(4) . . ? C30 C31 C32 103.6(3) . . ? O2 C32 C31 107.1(3) . . ? O3 C33 C34 105.9(4) . . ? C35 C34 C33 106.1(5) . . ? C35 C34 C35A 36.2(5) . . ? C33 C34 C35A 101.3(4) . . ? C34 C35 C36 102.5(6) . . ? C36 C35A C34 101.2(6) . . ? C35A C36 O3 115.1(6) . . ? C35A C36 C35 38.9(5) . . ? O3 C36 C35 102.9(4) . . ? O4 C37 C38 105.1(3) . . ? C37 C38 C39 103.2(3) . . ? C40 C39 C38 101.9(3) . . ? O4 C40 C39 105.6(3) . . ? O5 C41 C42 104.0(3) . . ? C43 C42 C41 102.8(3) . . ? C42 C43 C44 103.1(3) . . ? O5 C44 C43 106.3(3) . . ? C4TA O1TA C1TA 91.8(18) . . ? C2TA C1TA O1TA 100.9(15) . . ? C3TA C2TA C1TA 113.0(9) . . ? C2TA C3TA C4TA 107.1(8) . . ? C3TA C4TA O1TA 116.2(15) . . ? C4TC O1TC C1TC 103.4(11) . . ? C2TC C1TC O1TC 104.8(14) . . ? C1TC C2TC C3TC 107.8(13) . . ? C4TC C3TC C2TC 107.9(11) . . ? C3TC C4TC O1TC 99.7(11) . . ? C4TB O1TB C1TB 104.7(9) . . ? O1TB C1TB C2TB 111.5(10) . . ? C3TB C2TB C1TB 104.8(12) . . ? C2TB C3TB C4TB 101.0(13) . . ? O1TB C4TB C3TB 113.8(11) . . ? C1TD O1TD C4TD 114.1(11) . . ? O1TD C1TD C2TD 106.5(12) . . ? C1TD C2TD C3TD 106.7(11) . . ? C4TD C3TD C2TD 104.9(13) . . ? C3TD C4TD O1TD 106.1(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.598 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.060 #==== END data_FO3236 _database_code_depnum_ccdc_archive 'CCDC 666451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H64 F6 I N3 O6.50 Sr2' _chemical_formula_weight 1155.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8189(9) _cell_length_b 13.0620(9) _cell_length_c 17.2294(9) _cell_angle_alpha 73.020(4) _cell_angle_beta 75.497(4) _cell_angle_gamma 72.879(3) _cell_volume 2593.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 2.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6412 _exptl_absorpt_correction_T_max 0.7043 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16428 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.1250 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11199 _reflns_number_gt 6488 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+5.4211P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11199 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.77118(6) 0.79714(5) 0.26751(4) 0.02801(17) Uani 1 1 d . . . Sr2 Sr 0.48470(5) 0.83621(5) 0.25826(4) 0.02442(17) Uani 1 1 d . . . I I 1.03630(5) 0.73500(6) 0.28864(4) 0.0602(2) Uani 1 1 d . . . F1 F 0.5013(4) 0.6636(3) 0.4038(2) 0.0380(10) Uani 1 1 d . . . F2 F 0.5923(4) 0.9123(4) 0.5101(3) 0.0574(13) Uani 1 1 d . . . F3 F 0.5783(3) 0.7916(3) 0.1002(2) 0.0359(10) Uani 1 1 d . . . F4 F 0.7555(4) 0.4467(3) 0.2472(3) 0.0496(12) Uani 1 1 d . . . F5 F 0.7397(4) 1.0811(3) 0.0311(2) 0.0441(11) Uani 1 1 d . . . F6 F 0.4562(4) 1.0561(3) 0.2661(2) 0.0406(10) Uani 1 1 d . . . O1 O 0.7914(5) 0.6308(5) 0.3943(4) 0.0584(17) Uani 1 1 d . B . O2 O 0.8822(4) 0.7871(4) 0.1165(3) 0.0411(13) Uani 1 1 d . D . O3 O 0.7888(5) 0.9805(4) 0.2850(3) 0.0431(13) Uani 1 1 d . . . O4 O 0.3881(4) 0.7022(3) 0.2346(3) 0.0338(12) Uani 1 1 d . . . O5 O 0.3097(4) 0.8710(4) 0.3728(3) 0.0350(11) Uani 1 1 d . . . O6 O 0.3436(4) 0.9642(4) 0.1676(3) 0.0393(12) Uani 1 1 d . . . N1 N 0.5864(5) 0.8434(4) 0.3712(3) 0.0291(13) Uani 1 1 d . . . H1A H 0.5739 0.9177 0.3698 0.035 Uiso 1 1 calc R . . N2 N 0.6605(5) 0.6728(4) 0.2404(3) 0.0261(12) Uani 1 1 d . . . H2A H 0.6530 0.6185 0.2889 0.031 Uiso 1 1 calc R . . N3 N 0.6324(5) 0.9460(4) 0.1690(3) 0.0281(13) Uani 1 1 d . . . H3B H 0.6530 0.9269 0.1184 0.034 Uiso 1 1 calc R . . C1 C 0.5482(6) 0.7948(5) 0.4499(4) 0.0287(15) Uani 1 1 d . . . C2 C 0.5038(6) 0.7006(5) 0.4707(4) 0.0313(16) Uani 1 1 d . . . C3 C 0.4616(7) 0.6485(6) 0.5478(5) 0.0414(19) Uani 1 1 d . . . H3A H 0.4336 0.5856 0.5559 0.050 Uiso 1 1 calc R . . C4 C 0.4601(8) 0.6885(7) 0.6141(5) 0.054(2) Uani 1 1 d . . . H4A H 0.4294 0.6542 0.6683 0.065 Uiso 1 1 calc R . . C5 C 0.5028(8) 0.7774(7) 0.6013(5) 0.055(2) Uani 1 1 d . . . H5A H 0.5028 0.8054 0.6463 0.065 Uiso 1 1 calc R . . C6 C 0.5459(7) 0.8260(6) 0.5219(4) 0.0377(18) Uani 1 1 d . . . C7 C 0.6718(6) 0.6233(5) 0.1785(4) 0.0286(15) Uani 1 1 d . . . C8 C 0.6312(6) 0.6826(5) 0.1038(4) 0.0286(15) Uani 1 1 d . . . C9 C 0.6396(6) 0.6404(6) 0.0380(4) 0.0378(18) Uani 1 1 d . . . H9A H 0.6114 0.6861 -0.0099 0.045 Uiso 1 1 calc R . . C10 C 0.6899(7) 0.5293(6) 0.0424(5) 0.046(2) Uani 1 1 d . . . H10A H 0.6979 0.4981 -0.0028 0.055 Uiso 1 1 calc R . . C11 C 0.7278(7) 0.4658(6) 0.1132(5) 0.045(2) Uani 1 1 d . . . H11A H 0.7612 0.3896 0.1176 0.054 Uiso 1 1 calc R . . C12 C 0.7179(6) 0.5111(6) 0.1771(4) 0.0355(17) Uani 1 1 d . . . C13 C 0.6024(6) 1.0585(5) 0.1519(4) 0.0290(16) Uani 1 1 d . . . C14 C 0.6534(7) 1.1308(6) 0.0839(4) 0.0356(18) Uani 1 1 d . . . C15 C 0.6233(7) 1.2440(5) 0.0685(4) 0.0374(18) Uani 1 1 d . . . H15A H 0.6621 1.2867 0.0220 0.045 Uiso 1 1 calc R . . C16 C 0.5377(7) 1.2951(6) 0.1203(5) 0.043(2) Uani 1 1 d . . . H16A H 0.5171 1.3731 0.1112 0.052 Uiso 1 1 calc R . . C17 C 0.4817(7) 1.2297(5) 0.1862(5) 0.0360(17) Uani 1 1 d . . . H17A H 0.4205 1.2634 0.2220 0.043 Uiso 1 1 calc R . . C18 C 0.5132(6) 1.1183(5) 0.2001(4) 0.0320(16) Uani 1 1 d . . . C19 C 0.8396(12) 0.5176(11) 0.3971(8) 0.103(4) Uiso 1 1 d . . . H19A H 0.9211 0.5013 0.3783 0.123 Uiso 0.50 1 calc PR A 1 H19B H 0.8044 0.4867 0.3670 0.123 Uiso 0.50 1 calc PR A 1 H19C H 0.7845 0.4882 0.3844 0.123 Uiso 0.50 1 d PR A 2 H19D H 0.9033 0.5141 0.3507 0.123 Uiso 0.50 1 d PR A 2 C20 C 0.8016(15) 0.4796(13) 0.5012(10) 0.044(4) Uiso 0.50 1 d P B 1 H20A H 0.7315 0.4555 0.5149 0.053 Uiso 0.50 1 calc PR B 1 H20B H 0.8595 0.4167 0.5242 0.053 Uiso 0.50 1 calc PR B 1 C21 C 0.787(2) 0.566(2) 0.5360(16) 0.093(7) Uiso 0.50 1 d P B 1 H21A H 0.7109 0.5858 0.5670 0.112 Uiso 0.50 1 calc PR B 1 H21B H 0.8409 0.5495 0.5732 0.112 Uiso 0.50 1 calc PR B 1 C20A C 0.875(3) 0.448(2) 0.4618(18) 0.111(9) Uiso 0.50 1 d P B 2 H20C H 0.9502 0.4022 0.4475 0.133 Uiso 0.50 1 calc PR B 2 H20D H 0.8236 0.3996 0.4917 0.133 Uiso 0.50 1 calc PR B 2 C21A C 0.874(3) 0.519(3) 0.506(2) 0.159(14) Uiso 0.50 1 d P B 2 H21C H 0.9520 0.5181 0.5053 0.191 Uiso 0.50 1 calc PR B 2 H21D H 0.8392 0.4935 0.5636 0.191 Uiso 0.50 1 calc PR B 2 C22 C 0.8072(9) 0.6474(10) 0.4688(6) 0.089(4) Uani 1 1 d . . . H22A H 0.8846 0.6531 0.4616 0.107 Uiso 0.50 1 calc PR B 1 H22B H 0.7574 0.7183 0.4783 0.107 Uiso 0.50 1 calc PR B 1 H22C H 0.7360 0.6703 0.5053 0.107 Uiso 0.50 1 d PR B 2 H22D H 0.8531 0.7010 0.4580 0.107 Uiso 0.50 1 d PR B 2 C23 C 0.9263(8) 0.6767(7) 0.1041(6) 0.058(2) Uani 1 1 d . . . H23A H 0.8841 0.6627 0.0689 0.070 Uiso 0.50 1 calc PR C 1 H23B H 0.9209 0.6219 0.1577 0.070 Uiso 0.50 1 calc PR C 1 H23C H 0.8675 0.6465 0.0975 0.070 Uiso 0.50 1 d PR C 2 H23D H 0.9619 0.6267 0.1507 0.070 Uiso 0.50 1 d PR C 2 C24 C 1.0448(15) 0.6679(14) 0.0631(11) 0.051(4) Uiso 0.50 1 d P D 1 H24A H 1.0947 0.6389 0.1042 0.061 Uiso 0.50 1 calc PR D 1 H24B H 1.0669 0.6198 0.0239 0.061 Uiso 0.50 1 calc PR D 1 C24A C 1.0130(18) 0.6939(17) 0.0229(13) 0.064(5) Uiso 0.50 1 d P D 2 H24C H 1.0767 0.6287 0.0237 0.077 Uiso 0.50 1 calc PR D 2 H24D H 0.9788 0.7052 -0.0255 0.077 Uiso 0.50 1 calc PR D 2 C25 C 1.0466(11) 0.7840(10) 0.0193(7) 0.090(4) Uiso 1 1 d . . . H25A H 1.1197 0.7978 0.0156 0.109 Uiso 0.50 1 calc PR D 1 H25B H 1.0316 0.8000 -0.0373 0.109 Uiso 0.50 1 calc PR D 1 H25C H 1.0610 0.8257 -0.0388 0.109 Uiso 0.50 1 d PR D 2 H25D H 1.1160 0.7620 0.0416 0.109 Uiso 0.50 1 d PR D 2 C26 C 0.9582(7) 0.8533(7) 0.0688(5) 0.047(2) Uani 1 1 d . D . H26A H 0.9903 0.8767 0.1054 0.056 Uiso 1 1 calc R . . H26B H 0.9198 0.9199 0.0322 0.056 Uiso 1 1 calc R . . C27 C 0.7894(9) 1.0094(8) 0.3581(6) 0.071(3) Uiso 1 1 d . . . H27A H 0.8413 0.9508 0.3907 0.085 Uiso 1 1 calc R . . H27B H 0.7143 1.0190 0.3924 0.085 Uiso 1 1 calc R . . C28 C 0.8260(10) 1.1160(8) 0.3322(6) 0.075(3) Uani 1 1 d . . . H28A H 0.7739 1.1710 0.3617 0.090 Uiso 1 1 calc R . . H28B H 0.9013 1.1038 0.3435 0.090 Uiso 1 1 calc R . . C29 C 0.8252(10) 1.1535(7) 0.2413(6) 0.069(3) Uani 1 1 d . . . H29A H 0.7517 1.1999 0.2300 0.083 Uiso 1 1 calc R . . H29B H 0.8826 1.1951 0.2123 0.083 Uiso 1 1 calc R . . C30 C 0.8505(9) 1.0476(7) 0.2169(5) 0.059(3) Uani 1 1 d . . . H30A H 0.8254 1.0587 0.1645 0.071 Uiso 1 1 calc R . . H30B H 0.9311 1.0130 0.2103 0.071 Uiso 1 1 calc R . . C31 C 0.3963(8) 0.5909(6) 0.2828(5) 0.046(2) Uani 1 1 d . . . H31A H 0.4728 0.5573 0.2936 0.055 Uiso 1 1 calc R . . H31B H 0.3450 0.5902 0.3364 0.055 Uiso 1 1 calc R . . C32 C 0.3681(13) 0.5293(8) 0.2379(7) 0.105(5) Uani 1 1 d . . . H32A H 0.2988 0.5065 0.2675 0.126 Uiso 1 1 calc R . . H32B H 0.4280 0.4622 0.2330 0.126 Uiso 1 1 calc R . . C33 C 0.3531(8) 0.5985(6) 0.1555(5) 0.053(2) Uani 1 1 d . . . H33A H 0.2851 0.5935 0.1410 0.063 Uiso 1 1 calc R . . H33B H 0.4176 0.5761 0.1132 0.063 Uiso 1 1 calc R . . C34 C 0.3435(7) 0.7139(6) 0.1621(5) 0.0394(18) Uani 1 1 d . . . H34A H 0.3863 0.7536 0.1121 0.047 Uiso 1 1 calc R . . H34B H 0.2649 0.7556 0.1679 0.047 Uiso 1 1 calc R . . C35 C 0.2369(6) 0.7974(6) 0.4095(5) 0.045(2) Uani 1 1 d . . . H35A H 0.2697 0.7345 0.4516 0.054 Uiso 1 1 calc R . . H35B H 0.2226 0.7687 0.3670 0.054 Uiso 1 1 calc R . . C36 C 0.1301(9) 0.8669(9) 0.4489(7) 0.078(3) Uiso 1 1 d . . . H36A H 0.0688 0.8776 0.4198 0.094 Uiso 1 1 calc R . . H36B H 0.1088 0.8307 0.5076 0.094 Uiso 1 1 calc R . . C37 C 0.1547(8) 0.9753(8) 0.4411(6) 0.059(2) Uani 1 1 d . . . H37A H 0.1208 1.0330 0.3967 0.071 Uiso 1 1 calc R . . H37B H 0.1264 0.9992 0.4935 0.071 Uiso 1 1 calc R . . C38 C 0.2786(7) 0.9527(7) 0.4205(5) 0.0443(19) Uani 1 1 d . . . H38A H 0.3031 1.0204 0.3879 0.053 Uiso 1 1 calc R . . H38B H 0.3114 0.9241 0.4712 0.053 Uiso 1 1 calc R . . C39 C 0.2253(7) 0.9913(6) 0.2008(5) 0.0430(19) Uani 1 1 d . . . H39A H 0.2087 1.0414 0.2381 0.052 Uiso 1 1 calc R . . H39B H 0.1997 0.9238 0.2319 0.052 Uiso 1 1 calc R . . C40 C 0.1707(7) 1.0464(7) 0.1276(5) 0.048(2) Uani 1 1 d . . . H40A H 0.0991 1.0984 0.1417 0.058 Uiso 1 1 calc R . . H40B H 0.1579 0.9919 0.1036 0.058 Uiso 1 1 calc R . . C41 C 0.2563(7) 1.1075(6) 0.0686(5) 0.044(2) Uani 1 1 d . . . H41A H 0.2471 1.1233 0.0105 0.052 Uiso 1 1 calc R . . H41B H 0.2506 1.1775 0.0826 0.052 Uiso 1 1 calc R . . C42 C 0.3640(6) 1.0272(6) 0.0828(4) 0.0400(18) Uani 1 1 d . . . H42A H 0.3877 0.9781 0.0442 0.048 Uiso 1 1 calc R . . H42B H 0.4227 1.0664 0.0748 0.048 Uiso 1 1 calc R . . O1T O 0.0482(15) 0.2729(14) 0.2794(10) 0.101(5) Uiso 0.50 1 d P . . C1T C 0.0530(17) 0.2826(15) 0.2022(11) 0.060(5) Uiso 0.50 1 d P . . H1TA H 0.1097 0.2200 0.1841 0.072 Uiso 0.50 1 calc PR . . H1TB H -0.0195 0.2808 0.1930 0.072 Uiso 0.50 1 calc PR . . C2T C 0.077(2) 0.373(2) 0.1601(16) 0.096(7) Uiso 0.50 1 d P . . H2TA H 0.0097 0.4333 0.1573 0.115 Uiso 0.50 1 calc PR . . H2TB H 0.1141 0.3664 0.1032 0.115 Uiso 0.50 1 calc PR . . C3T C 0.1519(18) 0.3936(16) 0.2012(12) 0.069(5) Uiso 0.50 1 d P . . H3TA H 0.2279 0.3809 0.1683 0.082 Uiso 0.50 1 calc PR . . H3TB H 0.1285 0.4718 0.2044 0.082 Uiso 0.50 1 calc PR . . C4T C 0.153(2) 0.330(2) 0.2764(17) 0.114(9) Uiso 0.50 1 d P . . H4TA H 0.1355 0.3725 0.3189 0.136 Uiso 0.50 1 calc PR . . H4TB H 0.2245 0.2742 0.2810 0.136 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.0270(4) 0.0289(3) 0.0314(4) -0.0085(3) -0.0070(3) -0.0086(3) Sr2 0.0270(4) 0.0214(3) 0.0272(3) -0.0069(2) -0.0053(3) -0.0078(3) I 0.0336(3) 0.0883(5) 0.0612(4) -0.0132(3) -0.0171(3) -0.0154(3) F1 0.052(3) 0.036(2) 0.032(2) -0.0079(17) -0.0055(19) -0.021(2) F2 0.080(4) 0.064(3) 0.046(3) -0.026(2) -0.010(3) -0.034(3) F3 0.046(3) 0.028(2) 0.035(2) -0.0082(16) -0.0095(19) -0.0071(19) F4 0.056(3) 0.030(2) 0.060(3) -0.012(2) -0.016(2) 0.000(2) F5 0.051(3) 0.039(2) 0.039(2) -0.0107(19) 0.005(2) -0.016(2) F6 0.048(3) 0.033(2) 0.037(2) -0.0100(18) 0.004(2) -0.012(2) O1 0.059(4) 0.051(4) 0.060(4) 0.003(3) -0.032(3) -0.004(3) O2 0.039(3) 0.042(3) 0.039(3) -0.011(2) -0.002(2) -0.008(3) O3 0.058(4) 0.040(3) 0.041(3) -0.011(2) -0.008(3) -0.026(3) O4 0.045(3) 0.026(3) 0.038(3) -0.007(2) -0.012(2) -0.017(2) O5 0.032(3) 0.046(3) 0.033(3) -0.018(2) 0.000(2) -0.015(2) O6 0.032(3) 0.040(3) 0.040(3) 0.000(2) -0.012(2) -0.005(2) N1 0.037(4) 0.026(3) 0.026(3) -0.009(2) -0.002(3) -0.011(3) N2 0.032(3) 0.019(3) 0.028(3) -0.007(2) -0.004(2) -0.006(2) N3 0.038(4) 0.019(3) 0.032(3) -0.008(2) -0.009(3) -0.008(3) C1 0.027(4) 0.027(3) 0.034(4) -0.009(3) -0.009(3) -0.004(3) C2 0.035(4) 0.030(4) 0.027(4) -0.002(3) -0.010(3) -0.006(3) C3 0.049(5) 0.034(4) 0.037(4) 0.008(3) -0.014(4) -0.015(4) C4 0.063(6) 0.066(6) 0.026(4) 0.008(4) -0.008(4) -0.023(5) C5 0.067(6) 0.067(6) 0.032(5) -0.016(4) -0.011(4) -0.014(5) C6 0.042(5) 0.038(4) 0.036(4) -0.014(3) -0.011(4) -0.005(4) C7 0.029(4) 0.024(3) 0.029(4) -0.004(3) 0.006(3) -0.013(3) C8 0.028(4) 0.022(3) 0.040(4) -0.012(3) -0.003(3) -0.011(3) C9 0.045(5) 0.040(4) 0.037(4) -0.015(3) -0.007(4) -0.017(4) C10 0.057(6) 0.042(5) 0.049(5) -0.024(4) -0.004(4) -0.019(4) C11 0.052(6) 0.033(4) 0.053(5) -0.017(4) 0.002(4) -0.016(4) C12 0.037(5) 0.031(4) 0.038(4) -0.008(3) -0.008(3) -0.006(3) C13 0.039(4) 0.022(3) 0.031(4) -0.007(3) -0.014(3) -0.007(3) C14 0.048(5) 0.032(4) 0.030(4) -0.001(3) -0.010(4) -0.020(4) C15 0.055(5) 0.025(4) 0.033(4) 0.002(3) -0.009(4) -0.017(4) C16 0.066(6) 0.022(4) 0.044(5) -0.004(3) -0.024(4) -0.005(4) C17 0.043(5) 0.025(4) 0.044(4) -0.012(3) -0.016(4) -0.004(3) C18 0.038(4) 0.027(4) 0.033(4) -0.010(3) -0.005(3) -0.008(3) C22 0.056(7) 0.124(10) 0.054(7) -0.002(6) -0.017(5) 0.013(7) C23 0.051(6) 0.040(5) 0.078(6) -0.022(4) 0.011(5) -0.013(4) C26 0.041(5) 0.049(5) 0.045(5) -0.008(4) 0.001(4) -0.013(4) C28 0.109(10) 0.059(6) 0.076(7) -0.028(5) -0.007(6) -0.042(6) C29 0.095(9) 0.038(5) 0.078(7) -0.006(5) -0.027(6) -0.021(5) C30 0.080(7) 0.057(6) 0.053(5) -0.006(4) -0.014(5) -0.038(5) C31 0.067(6) 0.032(4) 0.041(5) -0.003(3) -0.011(4) -0.019(4) C32 0.211(15) 0.040(5) 0.102(9) -0.001(5) -0.107(10) -0.037(7) C33 0.081(7) 0.039(5) 0.052(5) -0.014(4) -0.017(5) -0.028(5) C34 0.045(5) 0.038(4) 0.044(4) -0.012(3) -0.012(4) -0.018(4) C35 0.033(5) 0.044(5) 0.053(5) -0.009(4) -0.002(4) -0.011(4) C37 0.055(6) 0.071(6) 0.047(5) -0.027(4) 0.000(4) -0.006(5) C38 0.043(5) 0.048(5) 0.047(5) -0.026(4) 0.001(4) -0.012(4) C39 0.044(5) 0.039(4) 0.039(4) -0.004(3) -0.004(4) -0.008(4) C40 0.041(5) 0.046(5) 0.050(5) -0.004(4) -0.011(4) -0.002(4) C41 0.048(5) 0.035(4) 0.042(5) 0.000(3) -0.011(4) -0.007(4) C42 0.032(4) 0.048(5) 0.039(4) -0.004(3) -0.007(3) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O3 2.579(5) . ? Sr1 O1 2.596(5) . ? Sr1 N1 2.614(6) . ? Sr1 N2 2.645(5) . ? Sr1 O2 2.654(5) . ? Sr1 N3 2.716(5) . ? Sr1 I 3.3414(9) . ? Sr1 Sr2 3.5935(9) . ? Sr2 O6 2.572(4) . ? Sr2 O4 2.590(4) . ? Sr2 O5 2.615(5) . ? Sr2 N3 2.620(5) . ? Sr2 N2 2.633(5) . ? Sr2 N1 2.635(5) . ? Sr2 F6 2.826(4) . ? Sr2 F3 2.841(4) . ? Sr2 F1 2.845(4) . ? F1 C2 1.384(7) . ? F2 C6 1.367(8) . ? F3 C8 1.376(7) . ? F4 C12 1.364(8) . ? F5 C14 1.375(9) . ? F6 C18 1.371(8) . ? O1 C19 1.417(13) . ? O1 C22 1.433(12) . ? O2 C26 1.433(9) . ? O2 C23 1.444(9) . ? O3 C27 1.419(10) . ? O3 C30 1.454(10) . ? O4 C31 1.436(8) . ? O4 C34 1.452(8) . ? O5 C38 1.438(8) . ? O5 C35 1.440(9) . ? O6 C39 1.455(9) . ? O6 C42 1.454(8) . ? N1 C1 1.353(8) . ? N2 C7 1.360(8) . ? N3 C13 1.365(8) . ? C1 C6 1.406(9) . ? C1 C2 1.420(9) . ? C2 C3 1.360(10) . ? C3 C4 1.382(11) . ? C4 C5 1.365(12) . ? C5 C6 1.378(11) . ? C7 C12 1.414(9) . ? C7 C8 1.430(9) . ? C8 C9 1.367(9) . ? C9 C10 1.392(10) . ? C10 C11 1.372(11) . ? C11 C12 1.358(10) . ? C13 C18 1.409(10) . ? C13 C14 1.423(9) . ? C14 C15 1.376(9) . ? C15 C16 1.368(11) . ? C16 C17 1.386(10) . ? C17 C18 1.356(9) . ? C19 C20A 1.30(3) . ? C19 C20 1.70(2) . ? C20 C21 1.38(3) . ? C21 C22 1.35(2) . ? C20A C21A 1.35(4) . ? C21A C22 1.66(4) . ? C23 C24 1.492(19) . ? C23 C24A 1.56(2) . ? C24 C25 1.487(19) . ? C24A C25 1.35(2) . ? C25 C26 1.481(14) . ? C27 C28 1.508(12) . ? C28 C29 1.500(13) . ? C29 C30 1.484(12) . ? C31 C32 1.431(11) . ? C32 C33 1.468(12) . ? C33 C34 1.510(10) . ? C35 C36 1.523(13) . ? C36 C37 1.500(13) . ? C37 C38 1.497(12) . ? C39 C40 1.489(10) . ? C40 C41 1.536(11) . ? C41 C42 1.494(10) . ? O1T C1T 1.29(2) . ? O1T C4T 1.70(3) . ? C1T C2T 1.27(3) . ? C2T C3T 1.45(3) . ? C3T C4T 1.32(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sr1 O1 116.30(17) . . ? O3 Sr1 N1 81.07(17) . . ? O1 Sr1 N1 76.29(19) . . ? O3 Sr1 N2 152.66(17) . . ? O1 Sr1 N2 78.45(17) . . ? N1 Sr1 N2 80.53(17) . . ? O3 Sr1 O2 103.97(16) . . ? O1 Sr1 O2 123.21(19) . . ? N1 Sr1 O2 151.54(16) . . ? N2 Sr1 O2 83.52(16) . . ? O3 Sr1 N3 78.69(15) . . ? O1 Sr1 N3 146.44(18) . . ? N1 Sr1 N3 76.90(17) . . ? N2 Sr1 N3 77.56(15) . . ? O2 Sr1 N3 76.73(16) . . ? O3 Sr1 I 78.38(13) . . ? O1 Sr1 I 74.36(14) . . ? N1 Sr1 I 131.37(12) . . ? N2 Sr1 I 128.88(12) . . ? O2 Sr1 I 76.68(11) . . ? N3 Sr1 I 139.19(12) . . ? O3 Sr1 Sr2 106.05(13) . . ? O1 Sr1 Sr2 99.97(14) . . ? N1 Sr1 Sr2 47.04(11) . . ? N2 Sr1 Sr2 46.94(12) . . ? O2 Sr1 Sr2 105.63(11) . . ? N3 Sr1 Sr2 46.54(12) . . ? I Sr1 Sr2 174.07(2) . . ? O6 Sr2 O4 76.61(15) . . ? O6 Sr2 O5 80.34(15) . . ? O4 Sr2 O5 83.88(15) . . ? O6 Sr2 N3 89.20(16) . . ? O4 Sr2 N3 135.36(16) . . ? O5 Sr2 N3 135.70(16) . . ? O6 Sr2 N2 135.59(16) . . ? O4 Sr2 N2 81.88(15) . . ? O5 Sr2 N2 135.43(16) . . ? N3 Sr2 N2 79.50(16) . . ? O6 Sr2 N1 139.22(17) . . ? O4 Sr2 N1 137.36(15) . . ? O5 Sr2 N1 82.21(16) . . ? N3 Sr2 N1 78.24(16) . . ? N2 Sr2 N1 80.38(17) . . ? O6 Sr2 F6 70.91(14) . . ? O4 Sr2 F6 143.78(14) . . ? O5 Sr2 F6 75.40(13) . . ? N3 Sr2 F6 60.56(15) . . ? N2 Sr2 F6 133.23(14) . . ? N1 Sr2 F6 69.13(14) . . ? O6 Sr2 F3 76.48(14) . . ? O4 Sr2 F3 70.81(13) . . ? O5 Sr2 F3 148.87(13) . . ? N3 Sr2 F3 64.73(14) . . ? N2 Sr2 F3 59.78(14) . . ? N1 Sr2 F3 128.76(15) . . ? F6 Sr2 F3 115.21(11) . . ? O6 Sr2 F1 141.52(14) . . ? O4 Sr2 F1 77.77(12) . . ? O5 Sr2 F1 68.78(14) . . ? N3 Sr2 F1 128.95(14) . . ? N2 Sr2 F1 66.99(14) . . ? N1 Sr2 F1 59.61(13) . . ? F6 Sr2 F1 119.82(11) . . ? F3 Sr2 F1 120.62(11) . . ? O6 Sr2 Sr1 137.96(11) . . ? O4 Sr2 Sr1 129.11(11) . . ? O5 Sr2 Sr1 128.68(10) . . ? N3 Sr2 Sr1 48.81(11) . . ? N2 Sr2 Sr1 47.24(11) . . ? N1 Sr2 Sr1 46.55(13) . . ? F6 Sr2 Sr1 86.62(9) . . ? F3 Sr2 Sr1 82.21(8) . . ? F1 Sr2 Sr1 80.45(9) . . ? C2 F1 Sr2 112.3(3) . . ? C8 F3 Sr2 113.1(3) . . ? C18 F6 Sr2 115.2(4) . . ? C19 O1 C22 105.3(8) . . ? C19 O1 Sr1 129.4(7) . . ? C22 O1 Sr1 118.8(6) . . ? C26 O2 C23 108.8(6) . . ? C26 O2 Sr1 125.1(4) . . ? C23 O2 Sr1 114.4(4) . . ? C27 O3 C30 107.2(6) . . ? C27 O3 Sr1 129.0(5) . . ? C30 O3 Sr1 118.5(4) . . ? C31 O4 C34 108.2(5) . . ? C31 O4 Sr2 123.2(4) . . ? C34 O4 Sr2 126.9(4) . . ? C38 O5 C35 107.0(6) . . ? C38 O5 Sr2 127.8(4) . . ? C35 O5 Sr2 124.4(4) . . ? C39 O6 C42 109.4(5) . . ? C39 O6 Sr2 121.5(4) . . ? C42 O6 Sr2 128.8(4) . . ? C1 N1 Sr1 133.6(4) . . ? C1 N1 Sr2 116.0(4) . . ? Sr1 N1 Sr2 86.40(16) . . ? C7 N2 Sr2 117.0(4) . . ? C7 N2 Sr1 134.1(4) . . ? Sr2 N2 Sr1 85.82(15) . . ? C13 N3 Sr2 118.6(5) . . ? C13 N3 Sr1 131.4(4) . . ? Sr2 N3 Sr1 84.66(14) . . ? N1 C1 C6 127.3(6) . . ? N1 C1 C2 122.7(6) . . ? C6 C1 C2 109.9(6) . . ? C3 C2 F1 119.0(6) . . ? C3 C2 C1 126.4(7) . . ? F1 C2 C1 114.6(5) . . ? C2 C3 C4 118.9(7) . . ? C5 C4 C3 119.6(7) . . ? C4 C5 C6 118.9(7) . . ? F2 C6 C5 118.4(7) . . ? F2 C6 C1 115.4(6) . . ? C5 C6 C1 126.2(7) . . ? N2 C7 C12 128.1(6) . . ? N2 C7 C8 121.8(6) . . ? C12 C7 C8 110.1(6) . . ? C9 C8 F3 118.7(6) . . ? C9 C8 C7 126.0(6) . . ? F3 C8 C7 115.3(5) . . ? C8 C9 C10 119.0(7) . . ? C11 C10 C9 118.6(7) . . ? C12 C11 C10 120.5(7) . . ? C11 C12 F4 119.8(6) . . ? C11 C12 C7 125.8(7) . . ? F4 C12 C7 114.4(6) . . ? N3 C13 C18 123.2(6) . . ? N3 C13 C14 125.8(7) . . ? C18 C13 C14 111.0(6) . . ? F5 C14 C15 119.0(6) . . ? F5 C14 C13 115.9(6) . . ? C15 C14 C13 125.0(7) . . ? C16 C15 C14 119.9(7) . . ? C15 C16 C17 118.1(7) . . ? C18 C17 C16 120.7(8) . . ? C17 C18 F6 119.2(7) . . ? C17 C18 C13 125.1(7) . . ? F6 C18 C13 115.6(6) . . ? C20A C19 O1 122.7(17) . . ? C20A C19 C20 38.7(15) . . ? O1 C19 C20 93.1(10) . . ? C21 C20 C19 110.5(15) . . ? C22 C21 C20 101.8(19) . . ? C19 C20A C21A 100(3) . . ? C20A C21A C22 113(3) . . ? C21 C22 O1 113.7(15) . . ? C21 C22 C21A 44.7(16) . . ? O1 C22 C21A 97.2(16) . . ? O2 C23 C24 107.1(9) . . ? O2 C23 C24A 102.5(9) . . ? C24 C23 C24A 31.4(8) . . ? C25 C24 C23 102.8(12) . . ? C25 C24A C23 106.3(15) . . ? C24A C25 C26 108.5(13) . . ? C24A C25 C24 33.5(9) . . ? C26 C25 C24 105.8(11) . . ? O2 C26 C25 106.7(7) . . ? O3 C27 C28 107.2(8) . . ? C29 C28 C27 104.2(8) . . ? C30 C29 C28 102.4(7) . . ? O3 C30 C29 103.7(8) . . ? C32 C31 O4 108.7(6) . . ? C31 C32 C33 109.0(7) . . ? C32 C33 C34 104.4(7) . . ? O4 C34 C33 106.5(6) . . ? O5 C35 C36 105.2(7) . . ? C37 C36 C35 105.8(8) . . ? C38 C37 C36 104.2(8) . . ? O5 C38 C37 104.1(6) . . ? O6 C39 C40 105.2(6) . . ? C39 C40 C41 102.1(6) . . ? C42 C41 C40 102.6(6) . . ? O6 C42 C41 105.7(6) . . ? C1T O1T C4T 101.4(17) . . ? C2T C1T O1T 110(2) . . ? C1T C2T C3T 107(2) . . ? C4T C3T C2T 112(2) . . ? C3T C4T O1T 97(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.966 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.128 #==== END data_FO3221 _database_code_depnum_ccdc_archive 'CCDC 666452' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Ba F4 N2 O2' _chemical_formula_weight 537.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3978(3) _cell_length_b 11.0772(4) _cell_length_c 11.9910(4) _cell_angle_alpha 103.658(2) _cell_angle_beta 93.466(2) _cell_angle_gamma 95.221(2) _cell_volume 1075.54(7) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7287 _exptl_absorpt_correction_T_max 0.7754 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7837 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4902 _reflns_number_gt 4192 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.6669P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4902 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba Ba 0.25712(2) 0.56580(2) 0.511940(18) 0.02181(9) Uani 1 1 d . . . F1 F -0.1185(4) 0.5074(3) 0.2949(2) 0.0495(7) Uani 1 1 d . . . F2 F 0.1859(4) 0.1680(3) 0.2594(3) 0.0605(9) Uani 1 1 d . . . F3 F 0.2097(3) 0.1687(3) 0.5805(3) 0.0521(7) Uani 1 1 d . . . F4 F 0.6201(3) 0.4995(3) 0.7103(2) 0.0416(6) Uani 1 1 d . . . O1 O 0.2182(4) 0.7492(3) 0.3915(3) 0.0474(9) Uani 1 1 d . . . O2 O 0.3466(4) 0.7558(4) 0.7103(3) 0.0622(11) Uani 1 1 d . . . N1 N 0.0316(4) 0.3555(3) 0.4027(3) 0.0309(8) Uani 1 1 d . . . N2 N 0.4271(4) 0.3552(3) 0.5294(3) 0.0291(7) Uani 1 1 d . . . C1 C 0.0361(4) 0.3407(4) 0.2863(3) 0.0288(9) Uani 1 1 d . . . C2 C -0.0370(5) 0.4179(4) 0.2284(4) 0.0351(10) Uani 1 1 d . . . C3 C -0.0377(7) 0.4123(5) 0.1122(4) 0.0510(13) Uani 1 1 d . . . H3A H -0.0896 0.4703 0.0798 0.061 Uiso 1 1 calc R . . C4 C 0.0386(7) 0.3206(6) 0.0444(4) 0.0546(14) Uani 1 1 d . . . H4A H 0.0405 0.3149 -0.0358 0.065 Uiso 1 1 calc R . . C5 C 0.1129(6) 0.2363(5) 0.0935(4) 0.0454(12) Uani 1 1 d . . . H5A H 0.1637 0.1711 0.0477 0.054 Uiso 1 1 calc R . . C6 C 0.1107(5) 0.2500(4) 0.2107(4) 0.0394(10) Uani 1 1 d . . . C7 C 0.4117(4) 0.3362(4) 0.6346(4) 0.0271(9) Uani 1 1 d . . . C8 C 0.3064(5) 0.2474(4) 0.6684(4) 0.0361(10) Uani 1 1 d . . . C9 C 0.2948(6) 0.2342(5) 0.7787(5) 0.0477(13) Uani 1 1 d . . . H9A H 0.2205 0.1708 0.7931 0.057 Uiso 1 1 calc R . . C10 C 0.3911(7) 0.3130(6) 0.8686(5) 0.0558(15) Uani 1 1 d . . . H10A H 0.3822 0.3057 0.9454 0.067 Uiso 1 1 calc R . . C11 C 0.5015(6) 0.4034(5) 0.8455(4) 0.0480(12) Uani 1 1 d . . . H11A H 0.5703 0.4585 0.9055 0.058 Uiso 1 1 calc R . . C12 C 0.5078(5) 0.4105(4) 0.7327(4) 0.0328(9) Uani 1 1 d . . . C13 C 0.2985(9) 0.8719(5) 0.4357(5) 0.0670(18) Uani 1 1 d . . . H13A H 0.4038 0.8684 0.4758 0.080 Uiso 1 1 calc R . . H13B H 0.2334 0.9232 0.4908 0.080 Uiso 1 1 calc R . . C14 C 0.3201(7) 0.9268(6) 0.3340(6) 0.0677(18) Uani 1 1 d . . . H14A H 0.3208 1.0188 0.3557 0.081 Uiso 1 1 calc R . . H14B H 0.4207 0.9054 0.2988 0.081 Uiso 1 1 calc R . . C15 C 0.1818(11) 0.8685(7) 0.2577(7) 0.106(3) Uani 1 1 d . . . H15A H 0.2051 0.8617 0.1766 0.128 Uiso 1 1 calc R . . H15B H 0.0903 0.9185 0.2738 0.128 Uiso 1 1 calc R . . C16 C 0.1426(6) 0.7419(5) 0.2779(5) 0.0522(14) Uani 1 1 d . . . H16A H 0.0250 0.7213 0.2754 0.063 Uiso 1 1 calc R . . H16B H 0.1859 0.6775 0.2191 0.063 Uiso 1 1 calc R . . C17 C 0.4327(8) 0.7375(7) 0.8104(6) 0.085(2) Uani 1 1 d . . . H17A H 0.5435 0.7196 0.7942 0.102 Uiso 1 1 calc R . . H17B H 0.3785 0.6668 0.8361 0.102 Uiso 1 1 calc R . . C18 C 0.4341(12) 0.8557(8) 0.8993(6) 0.120(4) Uani 1 1 d . . . H18A H 0.4229 0.8384 0.9760 0.144 Uiso 1 1 calc R . . H18B H 0.5361 0.9092 0.9026 0.144 Uiso 1 1 calc R . . C19 C 0.3021(8) 0.9166(6) 0.8679(5) 0.0648(16) Uani 1 1 d . . . H19A H 0.3245 1.0085 0.8957 0.078 Uiso 1 1 calc R . . H19B H 0.2029 0.8884 0.8993 0.078 Uiso 1 1 calc R . . C20 C 0.2876(8) 0.8771(5) 0.7378(5) 0.0579(15) Uani 1 1 d . . . H20A H 0.1745 0.8715 0.7068 0.070 Uiso 1 1 calc R . . H20B H 0.3532 0.9373 0.7054 0.070 Uiso 1 1 calc R . . H1N2 H 0.370(8) 0.296(7) 0.480(6) 0.087 Uiso 1 1 d . . . H1N1 H 0.049(8) 0.277(7) 0.418(6) 0.087 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba 0.01946(12) 0.02272(13) 0.02312(13) 0.00419(9) 0.00573(8) 0.00262(8) F1 0.0631(18) 0.0460(17) 0.0516(17) 0.0221(14) 0.0259(14) 0.0293(14) F2 0.072(2) 0.0515(19) 0.067(2) 0.0155(16) 0.0226(17) 0.0367(17) F3 0.0417(15) 0.0405(17) 0.074(2) 0.0171(15) 0.0083(14) -0.0083(13) F4 0.0394(14) 0.0446(16) 0.0353(14) 0.0008(12) 0.0123(11) -0.0064(12) O1 0.051(2) 0.048(2) 0.055(2) 0.0280(17) 0.0146(17) 0.0187(16) O2 0.0397(19) 0.079(3) 0.047(2) -0.023(2) 0.0045(17) -0.0034(19) N1 0.0310(18) 0.032(2) 0.0281(18) 0.0034(15) 0.0014(15) 0.0037(15) N2 0.0251(17) 0.0301(19) 0.0318(18) 0.0059(15) 0.0025(14) 0.0053(14) C1 0.0155(17) 0.035(2) 0.031(2) -0.0017(17) 0.0065(15) -0.0014(15) C2 0.034(2) 0.037(2) 0.036(2) 0.0066(19) 0.0151(19) 0.0101(19) C3 0.064(3) 0.062(4) 0.033(3) 0.018(2) 0.011(2) 0.016(3) C4 0.057(3) 0.079(4) 0.029(2) 0.013(3) 0.015(2) 0.006(3) C5 0.046(3) 0.050(3) 0.036(2) -0.002(2) 0.016(2) 0.004(2) C6 0.036(2) 0.040(3) 0.041(3) 0.005(2) 0.008(2) 0.008(2) C7 0.0170(17) 0.026(2) 0.046(2) 0.0186(18) 0.0124(17) 0.0099(15) C8 0.027(2) 0.034(2) 0.054(3) 0.019(2) 0.008(2) 0.0079(18) C9 0.044(3) 0.050(3) 0.066(3) 0.037(3) 0.026(3) 0.019(2) C10 0.052(3) 0.084(4) 0.047(3) 0.038(3) 0.021(3) 0.024(3) C11 0.044(3) 0.068(4) 0.037(3) 0.017(3) 0.012(2) 0.015(3) C12 0.031(2) 0.041(3) 0.030(2) 0.0101(19) 0.0128(18) 0.0093(19) C13 0.119(5) 0.036(3) 0.048(3) 0.009(2) -0.004(3) 0.027(3) C14 0.063(4) 0.053(4) 0.092(5) 0.035(3) -0.010(3) -0.006(3) C15 0.139(7) 0.080(5) 0.101(6) 0.058(5) -0.051(6) -0.039(5) C16 0.042(3) 0.051(3) 0.067(4) 0.029(3) -0.013(3) 0.002(2) C17 0.055(4) 0.076(5) 0.094(5) -0.033(4) -0.029(4) 0.024(3) C18 0.186(10) 0.082(6) 0.067(5) -0.038(4) -0.054(6) 0.072(6) C19 0.084(4) 0.057(4) 0.045(3) -0.004(3) -0.004(3) 0.010(3) C20 0.077(4) 0.045(3) 0.046(3) 0.009(3) 0.002(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba O1 2.787(3) . ? Ba O2 2.789(4) . ? Ba N1 2.820(4) 2_566 ? Ba N2 2.826(4) 2_666 ? Ba N1 2.861(4) . ? Ba F4 2.871(3) 2_666 ? Ba N2 2.885(3) . ? Ba F1 2.901(3) 2_566 ? Ba Ba 4.4005(4) 2_566 ? Ba Ba 4.4580(4) 2_666 ? F1 C2 1.380(5) . ? F1 Ba 2.901(3) 2_566 ? F2 C6 1.370(5) . ? F3 C8 1.365(6) . ? F4 C12 1.386(5) . ? F4 Ba 2.871(3) 2_666 ? O1 C13 1.427(7) . ? O1 C16 1.449(6) . ? O2 C17 1.429(8) . ? O2 C20 1.446(7) . ? N1 C1 1.370(5) . ? N1 Ba 2.820(4) 2_566 ? N1 H1N1 0.95(7) . ? N2 C7 1.339(5) . ? N2 Ba 2.826(3) 2_666 ? N2 H1N2 0.86(7) . ? C1 C2 1.383(6) . ? C1 C6 1.406(6) . ? C2 C3 1.380(6) . ? C3 C4 1.377(8) . ? C3 H3A 0.9500 . ? C4 C5 1.389(8) . ? C4 H4A 0.9500 . ? C5 C6 1.378(7) . ? C5 H5A 0.9500 . ? C7 C8 1.410(6) . ? C7 C12 1.421(6) . ? C8 C9 1.373(7) . ? C9 C10 1.379(8) . ? C9 H9A 0.9500 . ? C10 C11 1.389(8) . ? C10 H10A 0.9500 . ? C11 C12 1.378(6) . ? C11 H11A 0.9500 . ? C13 C14 1.498(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.435(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.490(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.480(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.425(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.512(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ba O2 88.48(12) . . ? O1 Ba N1 81.41(10) . 2_566 ? O2 Ba N1 74.08(10) . 2_566 ? O1 Ba N2 75.90(10) . 2_666 ? O2 Ba N2 79.15(11) . 2_666 ? N1 Ba N2 145.13(10) 2_566 2_666 ? O1 Ba N1 106.74(11) . . ? O2 Ba N1 146.15(11) . . ? N1 Ba N1 78.48(11) 2_566 . ? N2 Ba N1 133.32(10) 2_666 . ? O1 Ba F4 68.77(9) . 2_666 ? O2 Ba F4 133.66(10) . 2_666 ? N1 Ba F4 136.08(9) 2_566 2_666 ? N2 Ba F4 56.84(9) 2_666 2_666 ? N1 Ba F4 80.15(9) . 2_666 ? O1 Ba N2 145.26(10) . . ? O2 Ba N2 107.82(12) . . ? N1 Ba N2 132.02(10) 2_566 . ? N2 Ba N2 77.37(11) 2_666 . ? N1 Ba N2 76.77(10) . . ? F4 Ba N2 78.15(9) 2_666 . ? O1 Ba F1 136.48(9) . 2_566 ? O2 Ba F1 71.46(11) . 2_566 ? N1 Ba F1 56.37(9) 2_566 2_566 ? N2 Ba F1 133.41(9) 2_666 2_566 ? N1 Ba F1 77.00(10) . 2_566 ? F4 Ba F1 150.25(8) 2_666 2_566 ? N2 Ba F1 78.27(9) . 2_566 ? O1 Ba Ba 95.25(7) . 2_566 ? O2 Ba Ba 111.36(8) . 2_566 ? N1 Ba Ba 39.58(7) 2_566 2_566 ? N2 Ba Ba 166.39(7) 2_666 2_566 ? N1 Ba Ba 38.90(7) . 2_566 ? F4 Ba Ba 110.51(5) 2_666 2_566 ? N2 Ba Ba 106.27(7) . 2_566 ? F1 Ba Ba 59.92(6) 2_566 2_566 ? O1 Ba Ba 112.17(7) . 2_666 ? O2 Ba Ba 94.51(8) . 2_666 ? N1 Ba Ba 162.42(7) 2_566 2_666 ? N2 Ba Ba 39.16(7) 2_666 2_666 ? N1 Ba Ba 106.66(7) . 2_666 ? F4 Ba Ba 61.35(5) 2_666 2_666 ? N2 Ba Ba 38.21(7) . 2_666 ? F1 Ba Ba 107.70(5) 2_566 2_666 ? Ba Ba Ba 142.880(11) 2_566 2_666 ? C2 F1 Ba 114.5(2) . 2_566 ? C12 F4 Ba 115.1(2) . 2_666 ? C13 O1 C16 108.4(4) . . ? C13 O1 Ba 119.7(3) . . ? C16 O1 Ba 131.4(3) . . ? C17 O2 C20 109.1(4) . . ? C17 O2 Ba 123.6(4) . . ? C20 O2 Ba 126.2(3) . . ? C1 N1 Ba 114.2(2) . 2_566 ? C1 N1 Ba 107.0(3) . . ? Ba N1 Ba 101.52(11) 2_566 . ? C1 N1 H1N1 107(4) . . ? Ba N1 H1N1 110(4) 2_566 . ? Ba N1 H1N1 118(4) . . ? C7 N2 Ba 114.7(2) . 2_666 ? C7 N2 Ba 107.6(2) . . ? Ba N2 Ba 102.63(11) 2_666 . ? C7 N2 H1N2 109(5) . . ? Ba N2 H1N2 120(5) 2_666 . ? Ba N2 H1N2 101(5) . . ? N1 C1 C2 121.8(4) . . ? N1 C1 C6 126.8(4) . . ? C2 C1 C6 111.4(4) . . ? C3 C2 F1 117.9(4) . . ? C3 C2 C1 126.5(4) . . ? F1 C2 C1 115.6(4) . . ? C4 C3 C2 118.4(5) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 118.1(5) . . ? C6 C5 H5A 121.0 . . ? C4 C5 H5A 121.0 . . ? F2 C6 C5 118.1(4) . . ? F2 C6 C1 116.0(4) . . ? C5 C6 C1 125.9(4) . . ? N2 C7 C8 129.0(4) . . ? N2 C7 C12 121.5(4) . . ? C8 C7 C12 109.6(4) . . ? F3 C8 C9 119.1(4) . . ? F3 C8 C7 114.8(4) . . ? C9 C8 C7 126.1(5) . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 117.8(5) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? C11 C12 F4 117.3(4) . . ? C11 C12 C7 127.5(4) . . ? F4 C12 C7 115.2(3) . . ? O1 C13 C14 106.4(5) . . ? O1 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? O1 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.6 . . ? C15 C14 C13 102.2(6) . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C14 C15 C16 107.2(5) . . ? C14 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? C14 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? O1 C16 C15 104.9(5) . . ? O1 C16 H16A 110.8 . . ? C15 C16 H16A 110.8 . . ? O1 C16 H16B 110.8 . . ? C15 C16 H16B 110.8 . . ? H16A C16 H16B 108.8 . . ? O2 C17 C18 105.6(5) . . ? O2 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? O2 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C19 C18 C17 107.0(6) . . ? C19 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? C19 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C18 C19 C20 103.3(6) . . ? C18 C19 H19A 111.1 . . ? C20 C19 H19A 111.1 . . ? C18 C19 H19B 111.1 . . ? C20 C19 H19B 111.1 . . ? H19A C19 H19B 109.1 . . ? O2 C20 C19 104.9(5) . . ? O2 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? O2 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.873 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.124